# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_BPB-KCB31
_database_code_depnum_ccdc_archive 'CCDC 1963358'
loop_
_audit_author_name
_audit_author_address
'Bamaprasad Bag'
;CSIR Institute of Minerals and Materials Chemistry Bhubaneswar
India
;
_audit_update_record             
;
2020-01-20 deposited with the CCDC.	2020-07-07 downloaded from the CCDC.
;
_audit_creation_date             2019-11-03
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_chemical_formula_moiety         'C37 H41 N5 O3'
_chemical_formula_sum            'C37 H41 N5 O3'
_chemical_formula_weight         603.77
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
C 0.00347 0.00161 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
O 0.01158 0.00611 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390
32.90890 0.250800013542
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.00653 0.00323 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.5290002823
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,y+1/2,-z+1/2
3 -x,-y,-z
4 x,-y-1/2,z-1/2

_symmetry_Int_Tables_number      14
_cell_length_a                   9.236(2)
_cell_length_b                   14.416(3)
_cell_length_c                   25.771(6)
_cell_angle_alpha                90
_cell_angle_beta                 95.167(7)
_cell_angle_gamma                90
_cell_volume                     3417.6(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4729
_cell_measurement_theta_min      2.61
_cell_measurement_theta_max      17.05
_exptl_crystal_description       Block
_exptl_crystal_colour            Colourless
_exptl_absorpt_coefficient_mu    0.076
_exptl_crystal_density_diffrn    1.1733
_exptl_crystal_F_000             1288.5414
_diffrn_reflns_av_R_equivalents  0.0502
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15532
_diffrn_reflns_theta_full        17.0519
_diffrn_reflns_theta_max         17.05
_diffrn_reflns_theta_min         1.59
_diffrn_ambient_temperature      293.15
_diffrn_measured_fraction_theta_full 0.9955
_diffrn_measured_fraction_theta_max 0.9955

# start Validation Reply Form
_vrf_THETM01_BPB-KCB31           
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: The resolution reported is the best which could be
obtained. The complete set of data were collected, but the very high 
angle data were omitted as those were dominated by noise. 
;
_vrf_PLAT088_BPB-KCB31           
;
PROBLEM: Poor Data / Parameter Ratio ....................       4.29 Note  
RESPONSE: This alert could have generated because of inclusion of solvant
 molecule (water) in the formula, but "squeezed" them from the structure. 
The solvent molecule (water) was found to be highly disordered.
;
_vrf_PLAT355_BPB-KCB31           
;
PROBLEM: Long   O-H (X0.82,N0.98A)  O3       - H3       .       1.15 Ang.  
RESPONSE: The H-atom was assigned based on observed fourier electron density,
was not constructed, and not refined over riding model. 
;
_vrf_PLAT340_BPB-KCB31           
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0134 Ang.  
RESPONSE: The crystal structure had disorders in both the covalent framework
and lattoce solvent molecule (Water). Despite of efforts to obtain good quality 
crystal data, the disorder remained. Therefore, the data was refined with 
squeezing it in PLATON software.    
;
_vrf_PLAT414_BPB-KCB31           
;
PROBLEM: Short Intra D-H..H-X       H1       ..H25A             1.86 Ang.  
RESPONSE:This alert was generated due to associated disorder in the molecule.
;
# end Validation Reply Form

_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              7
_reflns_limit_h_min              -7
_reflns_limit_k_max              11
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                1732
_reflns_number_total             2005
_reflns_threshold_expression     I>=2u(I)
_computing_data_collection       'BRUKER APEX2'
_computing_cell_refinement       'BRUKER SAINT'
_computing_data_reduction        'BRUKER SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'ORTEP 3 and DIAMOND 3.0'
_computing_structure_refinement  'SHELXL-2013 and olex2.refine'
_refine_diff_density_max         0.2336
_refine_diff_density_min         -0.2557
_refine_diff_density_rms         0.0472
_refine_ls_d_res_high            1.2119
_refine_ls_d_res_low             12.8331
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.1554
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    37
_refine_ls_number_parameters     467
_refine_ls_number_reflns         2005
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0570
_refine_ls_restrained_S_all      1.1554
_refine_ls_shift/su_max          0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0808P)²+3.6964P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1529
_refine_ls_wR_factor_ref         0.1591

_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
3. Uiso/Uaniso restraints and constraints
: with sigma of 0.1 and sigma for terminal atoms of 0.2
4.a Secondary CH2 refined with riding coordinates:
 C21(H21a,H21b), C23(H23a,H23b), C36(H36a,H36b)
4.b Me refined with riding coordinates:
 C22(H22a,H22b,H22c), C24(H24a,H24b,H24c), C25(H25a,H25b,H25c), C26(H26a,H26b,
 H26c), C35(H35a,H35b,H35c), C37(H37a,H37b,H37c)
4.c Aromatic/amide H refined with riding coordinates:
 C1(H1a), C4(H4)
;
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_refinement_flags_posn
O1 O 1.0261(8) 0.0692(3) 0.35338(16) 0.0615(13) Uani 1.000000 .
O2 O 0.8027(5) 0.4315(4) 0.22959(16) 0.0743(15) Uani 1.000000 .
O3 O 0.7212(4) 0.4922(3) 0.3584(2) 0.0575(12) Uani 1.000000 .
N1 N 0.5550(10) -0.0619(6) 0.3209(3) 0.083(2) Uani 1.000000 .
N2 N 1.5070(10) 0.1748(5) 0.3987(3) 0.072(2) Uani 1.000000 .
N3 N 0.9010(5) 0.3117(4) 0.2810(3) 0.0453(14) Uani 1.000000 .
N4 N 0.8578(5) 0.3533(3) 0.3246(4) 0.0471(14) Uani 1.000000 .
N5 N 0.7195(7) 0.5318(5) 0.5402(3) 0.0757(17) Uani 1.000000 .
C1 C 0.7164(11) 0.1414(5) 0.2639(2) 0.0473(16) Uani 1.000000 .
H1a H 0.6906(11) 0.1869(5) 0.2391(2) 0.057(2) Uiso 1.000000 R
C2 C 0.6137(7) 0.0764(6) 0.2738(3) 0.0495(17) Uani 1.000000 .
C3 C 0.6530(12) 0.0056(6) 0.3103(3) 0.0565(18) Uani 1.000000 .
C4 C 0.7918(14) 0.0061(5) 0.3348(3) 0.0602(19) Uani 1.000000 .
H4 H 0.8197(14) -0.0402(5) 0.3587(3) 0.072(2) Uiso 1.000000 R
C5 C 1.2227(12) 0.2659(6) 0.3031(3) 0.0485(17) Uani 1.000000 .
C6 C 1.3558(10) 0.2577(6) 0.3307(4) 0.0508(18) Uani 1.000000 .
C7 C 1.3777(11) 0.1850(7) 0.3676(3) 0.053(2) Uani 1.000000 .
C8 C 1.2643(14) 0.1250(6) 0.3726(3) 0.055(2) Uani 1.000000 .
C9 C 0.8570(9) 0.1435(5) 0.2886(3) 0.0420(16) Uani 1.000000 .
C10 C 0.8912(10) 0.0748(6) 0.3244(3) 0.0510(17) Uani 1.000000 .
C11 C 1.1075(8) 0.2048(6) 0.3084(3) 0.0424(17) Uani 1.000000 .
C12 C 1.1309(12) 0.1336(6) 0.3438(3) 0.0472(17) Uani 1.000000 .
C13 C 0.9653(9) 0.2164(5) 0.2756(3) 0.0399(16) Uani 1.000000 .
C14 C 0.9874(8) 0.2200(7) 0.2182(3) 0.0429(17) Uani 1.000000 .
C15 C 1.0552(8) 0.1570(7) 0.1888(5) 0.0576(19) Uani 1.000000 .
C16 C 1.0625(9) 0.1774(8) 0.1365(5) 0.067(3) Uani 1.000000 .
C17 C 1.0053(10) 0.2568(8) 0.1139(4) 0.066(2) Uani 1.000000 .
C18 C 0.9369(8) 0.3196(6) 0.1431(5) 0.0572(18) Uani 1.000000 .
C19 C 0.9292(7) 0.2997(6) 0.1950(4) 0.0472(17) Uani 1.000000 .
C20 C 0.8694(7) 0.3581(6) 0.2346(4) 0.0506(17) Uani 1.000000 .
C21 C 0.5940(9) -0.1424(7) 0.3537(5) 0.142(4) Uani 1.000000 .
H21a H 0.6587(9) -0.1815(7) 0.3357(5) 0.171(5) Uiso 1.000000 R
H21b H 0.6476(9) -0.1209(7) 0.3855(5) 0.171(5) Uiso 1.000000 R
C22 C 0.4782(14) -0.1957(8) 0.3668(5) 0.202(5) Uani 1.000000 .
H22a H 0.5139(14) -0.2467(8) 0.3882(5) 0.302(7) Uiso 1.000000 R
H22b H 0.4146(14) -0.1583(8) 0.3856(5) 0.302(7) Uiso 1.000000 R
H22c H 0.4257(14) -0.2190(8) 0.3356(5) 0.302(7) Uiso 1.000000 R
C23 C 1.5380(8) 0.1017(5) 0.4361(3) 0.096(2) Uani 1.000000 .
H23a H 1.4604(8) 0.0987(5) 0.4590(3) 0.115(3) Uiso 1.000000 R
H23b H 1.5404(8) 0.0429(5) 0.4178(3) 0.115(3) Uiso 1.000000 R
C24 C 1.6767(11) 0.1150(6) 0.4676(4) 0.163(4) Uani 1.000000 .
H24a H 1.6924(11) 0.0647(6) 0.4918(4) 0.244(6) Uiso 1.000000 R
H24b H 1.7543(11) 0.1167(6) 0.4452(4) 0.244(6) Uiso 1.000000 R
H24c H 1.6743(11) 0.1725(6) 0.4864(4) 0.244(6) Uiso 1.000000 R
C25 C 0.4653(7) 0.0795(4) 0.2456(2) 0.074(2) Uani 1.000000 .
H25a H 0.4080(7) 0.0293(4) 0.2573(2) 0.111(3) Uiso 1.000000 R
H25b H 0.4198(7) 0.1375(4) 0.2526(2) 0.111(3) Uiso 1.000000 R
H25c H 0.4729(7) 0.0736(4) 0.2088(2) 0.111(3) Uiso 1.000000 R
C26 C 1.4791(7) 0.3220(5) 0.3229(2) 0.077(2) Uani 1.000000 .
H26a H 1.5624(7) 0.3048(5) 0.3458(2) 0.115(3) Uiso 1.000000 R
H26b H 1.5027(7) 0.3182(5) 0.2874(2) 0.115(3) Uiso 1.000000 R
H26c H 1.4513(7) 0.3844(5) 0.3304(2) 0.115(3) Uiso 1.000000 R
C27 C 0.8831(7) 0.3205(5) 0.3708(5) 0.0511(19) Uani 1.000000 .
C28 C 0.8363(7) 0.3731(6) 0.4140(4) 0.0469(17) Uani 1.000000 .
C29 C 0.7596(7) 0.4569(6) 0.4062(4) 0.0451(16) Uani 1.000000 .
C30 C 0.7187(7) 0.5069(6) 0.4473(5) 0.0545(18) Uani 1.000000 .
C31 C 0.8704(7) 0.3460(6) 0.4656(5) 0.0602(19) Uani 1.000000 .
C32 C 0.8342(8) 0.3961(7) 0.5071(4) 0.065(2) Uani 1.000000 .
C33 C 0.7564(8) 0.4799(6) 0.4991(4) 0.0588(18) Uani 1.000000 .
C34 C 0.6336(10) 0.6156(6) 0.5326(3) 0.077(2) Uani 1.000000 .
C35 C 0.7218(8) 0.6978(5) 0.5191(3) 0.103(2) Uani 1.000000 .
H35a H 0.6599(8) 0.7512(5) 0.5145(3) 0.155(4) Uiso 1.000000 R
H35b H 0.7963(8) 0.7093(5) 0.5468(3) 0.155(4) Uiso 1.000000 R
H35c H 0.7657(8) 0.6857(5) 0.4875(3) 0.155(4) Uiso 1.000000 R
C36 C 0.7836(8) 0.5146(5) 0.5937(3) 0.094(2) Uani 1.000000 .
H36a H 0.8808(8) 0.4896(5) 0.5927(3) 0.113(3) Uiso 1.000000 R
H36b H 0.7911(8) 0.5727(5) 0.6128(3) 0.113(3) Uiso 1.000000 R
C37 C 0.6941(8) 0.4488(6) 0.6208(3) 0.119(3) Uani 1.000000 .
H37a H 0.7379(8) 0.4387(6) 0.6556(3) 0.178(4) Uiso 1.000000 R
H37b H 0.5983(8) 0.4740(6) 0.6223(3) 0.178(4) Uiso 1.000000 R
H37c H 0.6879(8) 0.3910(6) 0.6023(3) 0.178(4) Uiso 1.000000 R
H34a H 0.544(7) 0.609(4) 0.504(2) 0.09(2) Uiso 1.000000 .
H5 H 1.213(6) 0.315(4) 0.276(2) 0.07(2) Uiso 1.000000 .
H8 H 1.268(5) 0.082(3) 0.3946(16) 0.011(18) Uiso 1.000000 .
H32 H 0.870(5) 0.374(4) 0.543(2) 0.07(2) Uiso 1.000000 .
H30 H 0.668(5) 0.566(4) 0.4408(19) 0.04(2) Uiso 1.000000 .
H34b H 0.581(7) 0.627(4) 0.565(3) 0.10(2) Uiso 1.000000 .
H17 H 1.003(6) 0.272(4) 0.077(3) 0.08(3) Uiso 1.000000 .
H2 H 1.576(6) 0.208(3) 0.3911(18) 0.03(2) Uiso 1.000000 .
H31 H 0.928(5) 0.287(4) 0.469(2) 0.06(2) Uiso 1.000000 .
H18 H 0.886(5) 0.379(4) 0.129(2) 0.06(2) Uiso 1.000000 .
H15 H 1.094(5) 0.106(4) 0.203(2) 0.04(2) Uiso 1.000000 .
H27 H 0.947(7) 0.265(5) 0.380(2) 0.09(3) Uiso 1.000000 .
H16 H 1.103(4) 0.136(3) 0.1200(19) 0.020(19) Uiso 1.000000 .
H3 H 0.775(8) 0.444(6) 0.330(3) 0.11(2) Uiso 1.000000 .
H1 H 0.476(6) -0.056(4) 0.308(2) 0.04(2) Uiso 1.000000 .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C10 1.397(7) . ?
O1 C12 1.380(7) . ?
O2 C20 1.226(8) . ?
O3 C29 1.349(7) . ?
O3 H3 1.15(9) . ?
N1 C3 1.373(9) . ?
N1 C21 1.460(10) . ?
N1 H1 0.77(5) . ?
N2 C7 1.385(8) . ?
N2 C23 1.439(9) . ?
N2 H2 0.84(5) . ?
N3 N4 1.365(6) . ?
N3 C13 1.508(7) . ?
N3 C20 1.377(7) . ?
N4 C27 1.283(7) . ?
N5 C33 1.366(8) . ?
N5 C34 1.450(9) . ?
N5 C36 1.471(8) . ?
C1 H1a 0.9300 . ?
C1 C2 1.375(7) . ?
C1 C9 1.394(8) . ?
C2 C3 1.413(8) . ?
C2 C25 1.493(8) . ?
C3 C4 1.377(8) . ?
C4 H4 0.9300 . ?
C4 C10 1.393(8) . ?
C5 C6 1.369(8) . ?
C5 C11 1.398(8) . ?
C5 H5 1.00(6) . ?
C6 C7 1.418(8) . ?
C6 C26 1.497(8) . ?
C7 C8 1.373(9) . ?
C8 C12 1.386(9) . ?
C8 H8 0.84(4) . ?
C9 C10 1.371(7) . ?
C9 C13 1.509(8) . ?
C11 C12 1.376(8) . ?
C11 C13 1.506(8) . ?
C13 C14 1.511(8) . ?
C14 C15 1.369(8) . ?
C14 C19 1.382(8) . ?
C15 C16 1.388(10) . ?
C15 H15 0.88(5) . ?
C16 C17 1.369(10) . ?
C16 H16 0.84(4) . ?
C17 C18 1.368(9) . ?
C17 H17 0.97(7) . ?
C18 C19 1.377(8) . ?
C18 H18 1.03(6) . ?
C19 C20 1.468(9) . ?
C21 H21a 0.9700 . ?
C21 H21b 0.9700 . ?
C21 C22 1.384(11) . ?
C22 H22a 0.9600 . ?
C22 H22b 0.9600 . ?
C22 H22c 0.9600 . ?
C23 H23a 0.9700 . ?
C23 H23b 0.9700 . ?
C23 C24 1.466(9) . ?
C24 H24a 0.9600 . ?
C24 H24b 0.9600 . ?
C24 H24c 0.9600 . ?
C25 H25a 0.9600 . ?
C25 H25b 0.9600 . ?
C25 H25c 0.9600 . ?
C26 H26a 0.9600 . ?
C26 H26b 0.9600 . ?
C26 H26c 0.9600 . ?
C27 C28 1.445(8) . ?
C27 H27 1.01(7) . ?
C28 C29 1.406(8) . ?
C28 C31 1.395(8) . ?
C29 C30 1.363(8) . ?
C30 C33 1.403(8) . ?
C30 H30 0.98(5) . ?
C31 C32 1.356(8) . ?
C31 H31 1.01(6) . ?
C32 C33 1.411(9) . ?
C32 H32 1.01(6) . ?
C34 C35 1.496(9) . ?
C34 H34a 1.06(6) . ?
C34 H34b 1.03(7) . ?
C35 H35a 0.9600 . ?
C35 H35b 0.9600 . ?
C35 H35c 0.9600 . ?
C36 H36a 0.9700 . ?
C36 H36b 0.9700 . ?
C36 C37 1.474(9) . ?
C37 H37a 0.9600 . ?
C37 H37b 0.9600 . ?
C37 H37c 0.9600 . ?

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
C12 O1 C10 118.1(6) . . ?
H3 O3 C29 105(3) . . ?
C21 N1 C3 123.0(8) . . ?
H1 N1 C3 117(5) . . ?
H1 N1 C21 120(5) . . ?
C23 N2 C7 125.1(7) . . ?
H2 N2 C7 116(4) . . ?
H2 N2 C23 118(3) . . ?
C13 N3 N4 128.6(6) . . ?
C20 N3 N4 116.5(6) . . ?
C20 N3 C13 114.6(6) . . ?
C27 N4 N3 124.0(6) . . ?
C34 N5 C33 121.5(7) . . ?
C36 N5 C33 121.9(7) . . ?
C36 N5 C34 115.9(7) . . ?
C2 C1 H1a 118.0(5) . . ?
C9 C1 H1a 118.0(4) . . ?
C9 C1 C2 124.0(5) . . ?
C3 C2 C1 118.5(6) . . ?
C25 C2 C1 120.5(8) . . ?
C25 C2 C3 121.0(9) . . ?
C2 C3 N1 120.7(9) . . ?
C4 C3 N1 121.1(9) . . ?
C4 C3 C2 118.2(7) . . ?
H4 C4 C3 119.4(5) . . ?
C10 C4 C3 121.3(6) . . ?
C10 C4 H4 119.4(5) . . ?
C11 C5 C6 123.4(7) . . ?
H5 C5 C6 117(3) . . ?
H5 C5 C11 120(3) . . ?
C7 C6 C5 118.7(6) . . ?
C26 C6 C5 122.3(9) . . ?
C26 C6 C7 119.0(10) . . ?
C6 C7 N2 122.0(10) . . ?
C8 C7 N2 120.3(10) . . ?
C8 C7 C6 117.7(8) . . ?
C12 C8 C7 122.8(8) . . ?
H8 C8 C7 123(3) . . ?
H8 C8 C12 114(3) . . ?
C10 C9 C1 116.1(6) . . ?
C13 C9 C1 121.5(8) . . ?
C13 C9 C10 122.4(8) . . ?
C4 C10 O1 115.3(9) . . ?
C9 C10 O1 122.9(8) . . ?
C9 C10 C4 121.8(7) . . ?
C12 C11 C5 117.3(7) . . ?
C13 C11 C5 120.5(9) . . ?
C13 C11 C12 122.1(9) . . ?
C8 C12 O1 116.6(9) . . ?
C11 C12 O1 123.3(9) . . ?
C11 C12 C8 120.1(8) . . ?
C9 C13 N3 109.8(6) . . ?
C11 C13 N3 112.4(6) . . ?
C11 C13 C9 111.1(6) . . ?
C14 C13 N3 98.5(5) . . ?
C14 C13 C9 113.0(6) . . ?
C14 C13 C11 111.4(6) . . ?
C15 C14 C13 128.8(8) . . ?
C19 C14 C13 111.7(8) . . ?
C19 C14 C15 119.5(7) . . ?
C16 C15 C14 117.5(8) . . ?
H15 C15 C14 122(3) . . ?
H15 C15 C16 121(3) . . ?
C17 C16 C15 122.7(9) . . ?
H16 C16 C15 114(3) . . ?
H16 C16 C17 123(3) . . ?
C18 C17 C16 119.9(8) . . ?
H17 C17 C16 125(4) . . ?
H17 C17 C18 115(4) . . ?
C19 C18 C17 117.6(8) . . ?
H18 C18 C17 125(3) . . ?
H18 C18 C19 117(3) . . ?
C18 C19 C14 122.8(8) . . ?
C20 C19 C14 109.4(8) . . ?
C20 C19 C18 127.8(10) . . ?
N3 C20 O2 125.2(7) . . ?
C19 C20 O2 129.6(9) . . ?
C19 C20 N3 105.2(7) . . ?
H21a C21 N1 108.5(5) . . ?
H21b C21 N1 108.5(5) . . ?
H21b C21 H21a 107.5 . . ?
C22 C21 N1 115.3(8) . . ?
C22 C21 H21a 108.5(6) . . ?
C22 C21 H21b 108.5(7) . . ?
H22a C22 C21 109.5 . . ?
H22b C22 C21 109.5 . . ?
H22b C22 H22a 109.5 . . ?
H22c C22 C21 109.5 . . ?
H22c C22 H22a 109.5 . . ?
H22c C22 H22b 109.5 . . ?
H23a C23 N2 109.1(4) . . ?
H23b C23 N2 109.1(4) . . ?
H23b C23 H23a 107.8 . . ?
C24 C23 N2 112.7(7) . . ?
C24 C23 H23a 109.1(5) . . ?
C24 C23 H23b 109.1(5) . . ?
H24a C24 C23 109.5 . . ?
H24b C24 C23 109.5 . . ?
H24b C24 H24a 109.5 . . ?
H24c C24 C23 109.5 . . ?
H24c C24 H24a 109.5 . . ?
H24c C24 H24b 109.5 . . ?
H25a C25 C2 109.5 . . ?
H25b C25 C2 109.5 . . ?
H25b C25 H25a 109.5 . . ?
H25c C25 C2 109.5 . . ?
H25c C25 H25a 109.5 . . ?
H25c C25 H25b 109.5 . . ?
H26a C26 C6 109.5 . . ?
H26b C26 C6 109.5 . . ?
H26b C26 H26a 109.5 . . ?
H26c C26 C6 109.5 . . ?
H26c C26 H26a 109.5 . . ?
H26c C26 H26b 109.5 . . ?
C28 C27 N4 118.6(8) . . ?
H27 C27 N4 125(3) . . ?
H27 C27 C28 116(3) . . ?
C29 C28 C27 121.5(9) . . ?
C31 C28 C27 122.0(9) . . ?
C31 C28 C29 116.5(8) . . ?
C28 C29 O3 122.9(9) . . ?
C30 C29 O3 116.2(8) . . ?
C30 C29 C28 120.9(8) . . ?
C33 C30 C29 122.1(8) . . ?
H30 C30 C29 119(3) . . ?
H30 C30 C33 119(3) . . ?
C32 C31 C28 123.4(7) . . ?
H31 C31 C28 113(3) . . ?
H31 C31 C32 124(3) . . ?
C33 C32 C31 120.0(7) . . ?
H32 C32 C31 119(3) . . ?
H32 C32 C33 121(3) . . ?
C30 C33 N5 121.9(9) . . ?
C32 C33 N5 121.0(10) . . ?
C32 C33 C30 117.1(8) . . ?
C35 C34 N5 112.9(7) . . ?
H34a C34 N5 114(3) . . ?
H34a C34 C35 109(3) . . ?
H34b C34 N5 109(3) . . ?
H34b C34 C35 112(3) . . ?
H34b C34 H34a 101(5) . . ?
H35a C35 C34 109.5 . . ?
H35b C35 C34 109.5 . . ?
H35b C35 H35a 109.5 . . ?
H35c C35 C34 109.5 . . ?
H35c C35 H35a 109.5 . . ?
H35c C35 H35b 109.5 . . ?
H36a C36 N5 109.5(4) . . ?
H36b C36 N5 109.5(4) . . ?
H36b C36 H36a 108.0 . . ?
C37 C36 N5 110.9(6) . . ?
C37 C36 H36a 109.5(4) . . ?
C37 C36 H36b 109.5(4) . . ?
H37a C37 C36 109.5 . . ?
H37b C37 C36 109.5 . . ?
H37b C37 H37a 109.5 . . ?
H37c C37 C36 109.5 . . ?
H37c C37 H37a 109.5 . . ?
H37c C37 H37b 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3 H3 N4 1.15(9) 1.53(9) 2.561(7) 146(5) .

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.109 -0.021 0.217 8.9 0.2 ?
2 0.000 0.000 0.500 107.4 16.5 ?
3 0.109 0.021 0.783 8.9 0.2 ?
4 0.000 0.500 0.000 107.4 16.5 ?
5 0.109 0.479 0.283 8.9 0.2 ?
6 -0.109 0.521 0.717 8.9 0.2 ?


_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
####################################################################### 
# 
# 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_BPB-KCB-76
_database_code_depnum_ccdc_archive 'CCDC 1978815'
loop_
_audit_author_name
_audit_author_address
'Bamaprasad Bag'
;CSIR Institute of Minerals and Materials Chemistry Bhubaneswar
India
;
_audit_update_record             
;
2020-01-20 deposited with the CCDC.	2020-07-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '[C33 H29 N3 O4). C2H5OH]'
_chemical_formula_sum            'C35 H35 N3 O5'
_chemical_formula_weight         577.66

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           9
_space_group_name_H-M_alt        'C c'
_space_group_name_Hall           'C -2yc'

_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, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   16.2392(19)
_cell_length_b                   12.0245(16)
_cell_length_c                   17.250(2)
_cell_angle_alpha                90
_cell_angle_beta                 110.696(3)
_cell_angle_gamma                90
_cell_volume                     3151.0(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    102(2)
_cell_measurement_reflns_used    3834
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      17.28

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_F_000             1224
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    0.082
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      102(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7413
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.250
_diffrn_reflns_theta_max         17.337
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.343
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.343
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_point_group_measured_fraction_full 0.330
_reflns_number_total             1882
_reflns_number_gt                1824
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.924
_reflns_Friedel_fraction_max     0.927
_reflns_Friedel_fraction_full    0.318

_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.
;
# start Validation Reply Form
_vrf_THETM01_BPB-KCB-76          
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: A full set of data was collected, however, the very high 
angle data was poor due to dominance by noise and therefore were omitted.
;
_vrf_PLAT089_BPB-KCB-76          
;
PROBLEM: Poor Data / Parameter Ratio (Zmax < 18) ........       2.44 Note  
RESPONSE: Even though complete set of crystal data were collected, the 
crystal (the largest available) still diffracted quite weakly at high 
angle. The data at high angle were omitted as those were dominated by noise.
;
_vrf_PLAT213_BPB-KCB-76          
;
PROBLEM: Atom C3              has ADP max/min Ratio .....        8.8 prolat
RESPONSE: This alert is generated due to disorder in the structure on 
account of the solvent molecule. Restraints were applied to disordered 
atoms. Several of the atoms were still not ideally shaped, however, this
does not indicate an incorrect atom-type assignment.
;
_vrf_PLAT340_BPB-KCB-76          
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.01362 Ang.  
RESPONSE: This alert is generated due to disorder in the structure on 
account of the solvent molecule. Restraints were applied to disordered 
atoms. Several of the atoms were still not ideally shaped, however, this
does not indicate an incorrect atom-type assignment.
;
# end Validation Reply Form

_computing_data_collection       'Bruker Apex 2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_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)+(0.0301P)²+0.4708P] 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     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 819 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.0(10)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1882
_refine_ls_number_parameters     400
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0278
_refine_ls_wR_factor_ref         0.0652
_refine_ls_wR_factor_gt          0.0639
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_restrained_S_all      1.076
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.002

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.4437(3) 0.8742(6) 0.4998(4) 0.0229(13) Uani 1 1 d . . . . .
O2 O 0.1599(3) 0.6836(4) 0.6317(3) 0.0227(13) Uani 1 1 d . . . . .
O3 O 0.5185(5) 1.1847(5) 0.6791(3) 0.0328(17) Uani 1 1 d . . . . .
O4 O 0.3704(4) 0.6247(5) 0.2794(5) 0.0365(17) Uani 1 1 d . . . . .
N1 N 0.2659(5) 0.7578(5) 0.5887(3) 0.0161(14) Uani 1 1 d . . . . .
N2 N 0.3225(6) 0.6719(5) 0.6275(3) 0.0186(16) Uani 1 1 d . . . . .
N3 N 0.8369(5) 0.3109(6) 0.8422(4) 0.0273(18) Uani 1 1 d . . . . .
C1 C 0.3287(5) 1.0089(8) 0.6229(5) 0.0203(19) Uani 1 1 d . . . . .
H1 H 0.2763 1.0035 0.6352 0.024 Uiso 1 1 calc R U . . .
C2 C 0.3867(6) 1.0921(7) 0.6592(4) 0.0219(19) Uani 1 1 d . . . . .
H2 H 0.3748 1.1437 0.6955 0.026 Uiso 1 1 calc R U . . .
C3 C 0.4636(6) 1.0993(8) 0.6416(5) 0.024(2) Uani 1 1 d . . . . .
C4 C 0.4810(5) 1.0249(10) 0.5890(6) 0.022(2) Uani 1 1 d . . . . .
H4 H 0.5343 1.0297 0.5780 0.026 Uiso 1 1 calc R U . . .
C5 C 0.2441(5) 0.7077(8) 0.4073(6) 0.0210(19) Uani 1 1 d . . . . .
H5 H 0.1887 0.6937 0.4124 0.025 Uiso 1 1 calc R U . . .
C6 C 0.2649(6) 0.6530(6) 0.3475(6) 0.024(2) Uani 1 1 d . . . . .
H6 H 0.2250 0.6008 0.3123 0.029 Uiso 1 1 calc R U . . .
C7 C 0.3457(7) 0.6748(8) 0.3386(6) 0.025(2) Uani 1 1 d . . . . .
C8 C 0.4030(5) 0.7476(8) 0.3906(7) 0.0217(19) Uani 1 1 d . . . . .
H8 H 0.4583 0.7616 0.3852 0.026 Uiso 1 1 calc R U . . .
C9 C 0.3427(6) 0.9315(7) 0.5686(5) 0.0142(18) Uani 1 1 d . . . . .
C10 C 0.4197(7) 0.9428(9) 0.5522(5) 0.021(2) Uani 1 1 d . . . . .
C11 C 0.3011(6) 0.7837(7) 0.4615(5) 0.014(2) Uani 1 1 d . . . . .
C12 C 0.3809(6) 0.8014(8) 0.4514(6) 0.0180(19) Uani 1 1 d . . . . .
C13 C 0.2775(5) 0.8414(7) 0.5285(5) 0.0153(19) Uani 1 1 d . . . . .
C14 C 0.1852(5) 0.8905(7) 0.4985(5) 0.0125(19) Uani 1 1 d . . . . .
C15 C 0.1537(6) 0.9759(7) 0.4435(4) 0.0174(19) Uani 1 1 d . . . . .
H15 H 0.1888 1.0081 0.4155 0.021 Uiso 1 1 calc R U . . .
C16 C 0.0689(6) 1.0144(5) 0.4297(4) 0.0261(19) Uani 1 1 d . . . . .
H16 H 0.0452 1.0721 0.3905 0.031 Uiso 1 1 calc R U . . .
C17 C 0.0183(5) 0.9701(7) 0.4722(5) 0.0244(19) Uani 1 1 d . . . . .
H17 H -0.0386 0.9995 0.4636 0.029 Uiso 1 1 calc R U . . .
C18 C 0.0505(6) 0.8830(7) 0.5272(5) 0.0188(19) Uani 1 1 d . . . . .
H18 H 0.0163 0.8514 0.5563 0.023 Uiso 1 1 calc R U . . .
C19 C 0.1338(6) 0.8436(7) 0.5385(5) 0.0165(19) Uani 1 1 d . . . . .
C20 C 0.1830(6) 0.7537(8) 0.5922(5) 0.015(2) Uani 1 1 d . . . . .
C21 C 0.4049(8) 0.6811(6) 0.6385(4) 0.020(2) Uani 1 1 d . . . . .
H21 H 0.4249 0.7470 0.6206 0.024 Uiso 1 1 calc R U . . .
C22 C 0.4671(7) 0.5961(7) 0.6766(4) 0.0184(19) Uani 1 1 d . . . . .
H22 H 0.4461 0.5272 0.6893 0.022 Uiso 1 1 calc R U . . .
C23 C 0.5543(8) 0.6090(6) 0.6955(5) 0.023(2) Uani 1 1 d . . . . .
H23 H 0.5720 0.6789 0.6812 0.028 Uiso 1 1 calc R U . . .
C24 C 0.6251(7) 0.5310(8) 0.7348(5) 0.0153(19) Uani 1 1 d . . . . .
C25 C 0.7121(8) 0.5661(7) 0.7617(5) 0.0199(18) Uani 1 1 d . . . . .
H25 H 0.7239 0.6420 0.7545 0.024 Uiso 1 1 calc R U . . .
C26 C 0.7814(5) 0.4963(10) 0.7978(4) 0.0210(19) Uani 1 1 d . . . . .
H26 H 0.8395 0.5253 0.8156 0.025 Uiso 1 1 calc R U . . .
C27 C 0.6118(5) 0.4180(9) 0.7471(4) 0.0204(19) Uani 1 1 d . . . . .
H27 H 0.5534 0.3899 0.7297 0.024 Uiso 1 1 calc R U . . .
C28 C 0.6806(7) 0.3472(6) 0.7833(5) 0.0205(19) Uani 1 1 d . . . . .
H28 H 0.6685 0.2716 0.7913 0.025 Uiso 1 1 calc R U . . .
C29 C 0.7688(7) 0.3831(9) 0.8094(5) 0.0195(19) Uani 1 1 d . . . . .
C30 C 0.8226(5) 0.1904(7) 0.8456(5) 0.032(2) Uani 1 1 d . . . . .
H30A H 0.8760 0.1504 0.8458 0.039 Uiso 1 1 calc R U . . .
H30B H 0.7732 0.1676 0.7953 0.039 Uiso 1 1 calc R U . . .
C31 C 0.8021(5) 0.1573(6) 0.9221(5) 0.042(2) Uani 1 1 d . . . . .
H31A H 0.7927 0.0767 0.9216 0.063 Uiso 1 1 calc R U . . .
H31B H 0.7489 0.1959 0.9217 0.063 Uiso 1 1 calc R U . . .
H31C H 0.8516 0.1778 0.9720 0.063 Uiso 1 1 calc R U . . .
C32 C 0.9268(5) 0.3502(6) 0.8836(5) 0.030(2) Uani 1 1 d . . . . .
H32A H 0.9568 0.3004 0.9308 0.036 Uiso 1 1 calc R U . . .
H32B H 0.9248 0.4254 0.9062 0.036 Uiso 1 1 calc R U . . .
C33 C 0.9804(5) 0.3551(6) 0.8272(5) 0.050(3) Uani 1 1 d . . . . .
H33A H 1.0399 0.3818 0.8586 0.075 Uiso 1 1 calc R U . . .
H33B H 0.9521 0.4059 0.7810 0.075 Uiso 1 1 calc R U . . .
H33C H 0.9838 0.2806 0.8054 0.075 Uiso 1 1 calc R U . . .
O5 O 0.2332(4) 0.5337(5) 0.1629(3) 0.0406(14) Uani 1 1 d . . . . .
C34 C 0.2187(6) 0.5822(7) 0.0833(5) 0.047(2) Uani 1 1 d . . . . .
H34A H 0.1785 0.5345 0.0394 0.056 Uiso 1 1 calc R U . . .
H34B H 0.2753 0.5877 0.0738 0.056 Uiso 1 1 calc R U . . .
C35 C 0.1794(6) 0.6955(7) 0.0795(5) 0.051(2) Uani 1 1 d . . . . .
H35A H 0.1697 0.7286 0.0251 0.076 Uiso 1 1 calc R U . . .
H35B H 0.2196 0.7426 0.1228 0.076 Uiso 1 1 calc R U . . .
H35C H 0.1231 0.6895 0.0882 0.076 Uiso 1 1 calc R U . . .
H3O H 0.563(4) 1.187(5) 0.674(4) 0.00(3) Uiso 1 1 d . . . . .
H4O H 0.335(4) 0.590(5) 0.247(4) 0.00(3) Uiso 1 1 d . . . . .
H5O H 0.238(5) 0.453(8) 0.163(5) 0.08(3) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C10 1.379(9) . ?
O1 C12 1.379(8) . ?
O2 C20 1.223(9) . ?
O3 C3 1.364(8) . ?
O3 H3O 0.75(6) . ?
O4 C7 1.361(9) . ?
O4 H4O 0.77(6) . ?
N1 C20 1.370(8) . ?
N1 N2 1.386(7) . ?
N1 C13 1.504(9) . ?
N2 C21 1.288(8) . ?
N3 C29 1.362(8) . ?
N3 C32 1.458(8) . ?
N3 C30 1.471(8) . ?
C1 C2 1.365(9) . ?
C1 C9 1.395(9) . ?
C1 H1 0.9500 . ?
C2 C3 1.387(9) . ?
C2 H2 0.9500 . ?
C3 C4 1.374(10) . ?
C4 C10 1.387(9) . ?
C4 H4 0.9500 . ?
C5 C6 1.363(9) . ?
C5 C11 1.397(9) . ?
C5 H5 0.9500 . ?
C6 C7 1.399(10) . ?
C6 H6 0.9500 . ?
C7 C8 1.360(9) . ?
C8 C12 1.382(10) . ?
C8 H8 0.9500 . ?
C9 C10 1.382(9) . ?
C9 C13 1.503(9) . ?
C11 C12 1.385(9) . ?
C11 C13 1.510(9) . ?
C13 C14 1.521(9) . ?
C14 C15 1.370(9) . ?
C14 C19 1.377(9) . ?
C15 C16 1.391(9) . ?
C15 H15 0.9500 . ?
C16 C17 1.387(10) . ?
C16 H16 0.9500 . ?
C17 C18 1.385(9) . ?
C17 H17 0.9500 . ?
C18 C19 1.381(9) . ?
C18 H18 0.9500 . ?
C19 C20 1.463(10) . ?
C21 C22 1.424(10) . ?
C21 H21 0.9500 . ?
C22 C23 1.345(9) . ?
C22 H22 0.9500 . ?
C23 C24 1.453(10) . ?
C23 H23 0.9500 . ?
C24 C25 1.388(9) . ?
C24 C27 1.403(9) . ?
C25 C26 1.365(8) . ?
C25 H25 0.9500 . ?
C26 C29 1.401(9) . ?
C26 H26 0.9500 . ?
C27 C28 1.367(9) . ?
C27 H27 0.9500 . ?
C28 C29 1.410(9) . ?
C28 H28 0.9500 . ?
C30 C31 1.523(10) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 C33 1.520(10) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
O5 C34 1.434(9) . ?
O5 H5O 0.97(9) . ?
C34 C35 1.497(9) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?

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
C10 O1 C12 117.2(7) . . ?
C3 O3 H3O 118(5) . . ?
C7 O4 H4O 116(5) . . ?
C20 N1 N2 116.5(6) . . ?
C20 N1 C13 114.7(7) . . ?
N2 N1 C13 127.4(7) . . ?
C21 N2 N1 118.9(6) . . ?
C29 N3 C32 121.4(7) . . ?
C29 N3 C30 121.8(7) . . ?
C32 N3 C30 116.4(7) . . ?
C2 C1 C9 123.2(6) . . ?
C2 C1 H1 118.4 . . ?
C9 C1 H1 118.4 . . ?
C1 C2 C3 118.3(7) . . ?
C1 C2 H2 120.9 . . ?
C3 C2 H2 120.9 . . ?
O3 C3 C4 123.3(10) . . ?
O3 C3 C2 115.6(10) . . ?
C4 C3 C2 121.1(7) . . ?
C3 C4 C10 118.9(7) . . ?
C3 C4 H4 120.6 . . ?
C10 C4 H4 120.6 . . ?
C6 C5 C11 122.7(7) . . ?
C6 C5 H5 118.7 . . ?
C11 C5 H5 118.7 . . ?
C5 C6 C7 119.0(7) . . ?
C5 C6 H6 120.5 . . ?
C7 C6 H6 120.5 . . ?
C8 C7 O4 117.8(10) . . ?
C8 C7 C6 119.8(7) . . ?
O4 C7 C6 122.4(10) . . ?
C7 C8 C12 120.2(8) . . ?
C7 C8 H8 119.9 . . ?
C12 C8 H8 119.9 . . ?
C10 C9 C1 116.4(7) . . ?
C10 C9 C13 121.2(9) . . ?
C1 C9 C13 122.3(8) . . ?
O1 C10 C9 124.2(9) . . ?
O1 C10 C4 113.7(9) . . ?
C9 C10 C4 122.2(8) . . ?
C12 C11 C5 116.4(7) . . ?
C12 C11 C13 121.9(8) . . ?
C5 C11 C13 121.7(9) . . ?
O1 C12 C8 115.0(9) . . ?
O1 C12 C11 123.1(9) . . ?
C8 C12 C11 121.9(8) . . ?
C9 C13 N1 113.8(6) . . ?
C9 C13 C11 110.8(7) . . ?
N1 C13 C11 110.4(6) . . ?
C9 C13 C14 109.0(7) . . ?
N1 C13 C14 98.4(6) . . ?
C11 C13 C14 113.9(7) . . ?
C15 C14 C19 120.7(7) . . ?
C15 C14 C13 127.5(9) . . ?
C19 C14 C13 111.7(8) . . ?
C14 C15 C16 118.2(6) . . ?
C14 C15 H15 120.9 . . ?
C16 C15 H15 120.9 . . ?
C17 C16 C15 121.2(7) . . ?
C17 C16 H16 119.4 . . ?
C15 C16 H16 119.4 . . ?
C18 C17 C16 120.2(7) . . ?
C18 C17 H17 119.9 . . ?
C16 C17 H17 119.9 . . ?
C19 C18 C17 118.0(7) . . ?
C19 C18 H18 121.0 . . ?
C17 C18 H18 121.0 . . ?
C14 C19 C18 121.7(8) . . ?
C14 C19 C20 109.1(8) . . ?
C18 C19 C20 129.1(10) . . ?
O2 C20 N1 123.2(8) . . ?
O2 C20 C19 131.0(9) . . ?
N1 C20 C19 105.8(8) . . ?
N2 C21 C22 122.5(7) . . ?
N2 C21 H21 118.7 . . ?
C22 C21 H21 118.7 . . ?
C23 C22 C21 122.9(7) . . ?
C23 C22 H22 118.5 . . ?
C21 C22 H22 118.5 . . ?
C22 C23 C24 129.1(7) . . ?
C22 C23 H23 115.5 . . ?
C24 C23 H23 115.5 . . ?
C25 C24 C27 115.9(7) . . ?
C25 C24 C23 120.3(9) . . ?
C27 C24 C23 123.9(9) . . ?
C26 C25 C24 122.9(7) . . ?
C26 C25 H25 118.5 . . ?
C24 C25 H25 118.5 . . ?
C25 C26 C29 121.6(7) . . ?
C25 C26 H26 119.2 . . ?
C29 C26 H26 119.2 . . ?
C28 C27 C24 121.9(7) . . ?
C28 C27 H27 119.1 . . ?
C24 C27 H27 119.1 . . ?
C27 C28 C29 121.9(7) . . ?
C27 C28 H28 119.0 . . ?
C29 C28 H28 119.0 . . ?
N3 C29 C26 122.8(9) . . ?
N3 C29 C28 121.5(9) . . ?
C26 C29 C28 115.8(8) . . ?
N3 C30 C31 112.2(6) . . ?
N3 C30 H30A 109.2 . . ?
C31 C30 H30A 109.2 . . ?
N3 C30 H30B 109.2 . . ?
C31 C30 H30B 109.2 . . ?
H30A C30 H30B 107.9 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N3 C32 C33 113.5(6) . . ?
N3 C32 H32A 108.9 . . ?
C33 C32 H32A 108.9 . . ?
N3 C32 H32B 108.9 . . ?
C33 C32 H32B 108.9 . . ?
H32A C32 H32B 107.7 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C34 O5 H5O 113(5) . . ?
O5 C34 C35 109.5(6) . . ?
O5 C34 H34A 109.8 . . ?
C35 C34 H34A 109.8 . . ?
O5 C34 H34B 109.8 . . ?
C35 C34 H34B 109.8 . . ?
H34A C34 H34B 108.2 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C20 N1 N2 C21 -168.2(5) . . . . ?
C13 N1 N2 C21 25.8(9) . . . . ?
C9 C1 C2 C3 -0.5(10) . . . . ?
C1 C2 C3 O3 179.4(6) . . . . ?
C1 C2 C3 C4 0.1(9) . . . . ?
O3 C3 C4 C10 -178.2(6) . . . . ?
C2 C3 C4 C10 1.0(9) . . . . ?
C11 C5 C6 C7 -1.2(10) . . . . ?
C5 C6 C7 C8 1.6(9) . . . . ?
C5 C6 C7 O4 -179.0(6) . . . . ?
O4 C7 C8 C12 179.5(6) . . . . ?
C6 C7 C8 C12 -1.0(9) . . . . ?
C2 C1 C9 C10 -0.2(9) . . . . ?
C2 C1 C9 C13 -179.3(6) . . . . ?
C12 O1 C10 C9 10.4(9) . . . . ?
C12 O1 C10 C4 -170.5(5) . . . . ?
C1 C9 C10 O1 -179.6(6) . . . . ?
C13 C9 C10 O1 -0.5(10) . . . . ?
C1 C9 C10 C4 1.4(9) . . . . ?
C13 C9 C10 C4 -179.5(6) . . . . ?
C3 C4 C10 O1 179.1(5) . . . . ?
C3 C4 C10 C9 -1.8(10) . . . . ?
C6 C5 C11 C12 0.1(9) . . . . ?
C6 C5 C11 C13 -178.6(6) . . . . ?
C10 O1 C12 C8 170.0(5) . . . . ?
C10 O1 C12 C11 -9.3(8) . . . . ?
C7 C8 C12 O1 -179.3(5) . . . . ?
C7 C8 C12 C11 0.0(9) . . . . ?
C5 C11 C12 O1 179.7(6) . . . . ?
C13 C11 C12 O1 -1.6(9) . . . . ?
C5 C11 C12 C8 0.5(9) . . . . ?
C13 C11 C12 C8 179.2(6) . . . . ?
C10 C9 C13 N1 115.7(8) . . . . ?
C1 C9 C13 N1 -65.3(9) . . . . ?
C10 C9 C13 C11 -9.4(9) . . . . ?
C1 C9 C13 C11 169.5(6) . . . . ?
C10 C9 C13 C14 -135.5(7) . . . . ?
C1 C9 C13 C14 43.5(9) . . . . ?
C20 N1 C13 C9 117.3(7) . . . . ?
N2 N1 C13 C9 -76.5(8) . . . . ?
C20 N1 C13 C11 -117.3(7) . . . . ?
N2 N1 C13 C11 48.9(9) . . . . ?
C20 N1 C13 C14 2.1(7) . . . . ?
N2 N1 C13 C14 168.3(5) . . . . ?
C12 C11 C13 C9 10.5(9) . . . . ?
C5 C11 C13 C9 -170.8(6) . . . . ?
C12 C11 C13 N1 -116.6(7) . . . . ?
C5 C11 C13 N1 62.1(9) . . . . ?
C12 C11 C13 C14 133.8(7) . . . . ?
C5 C11 C13 C14 -47.5(9) . . . . ?
C9 C13 C14 C15 58.6(9) . . . . ?
N1 C13 C14 C15 177.5(6) . . . . ?
C11 C13 C14 C15 -65.7(10) . . . . ?
C9 C13 C14 C19 -116.9(6) . . . . ?
N1 C13 C14 C19 1.9(7) . . . . ?
C11 C13 C14 C19 118.7(7) . . . . ?
C19 C14 C15 C16 0.5(9) . . . . ?
C13 C14 C15 C16 -174.7(6) . . . . ?
C14 C15 C16 C17 1.9(9) . . . . ?
C15 C16 C17 C18 -2.5(9) . . . . ?
C16 C17 C18 C19 0.6(9) . . . . ?
C15 C14 C19 C18 -2.4(9) . . . . ?
C13 C14 C19 C18 173.5(6) . . . . ?
C15 C14 C19 C20 179.1(5) . . . . ?
C13 C14 C19 C20 -5.0(7) . . . . ?
C17 C18 C19 C14 1.8(8) . . . . ?
C17 C18 C19 C20 -180.0(6) . . . . ?
N2 N1 C20 O2 5.0(8) . . . . ?
C13 N1 C20 O2 172.7(6) . . . . ?
N2 N1 C20 C19 -172.8(5) . . . . ?
C13 N1 C20 C19 -5.1(7) . . . . ?
C14 C19 C20 O2 -171.5(6) . . . . ?
C18 C19 C20 O2 10.1(11) . . . . ?
C14 C19 C20 N1 6.1(7) . . . . ?
C18 C19 C20 N1 -172.3(6) . . . . ?
N1 N2 C21 C22 -179.0(5) . . . . ?
N2 C21 C22 C23 -173.5(6) . . . . ?
C21 C22 C23 C24 179.3(6) . . . . ?
C22 C23 C24 C25 -169.2(7) . . . . ?
C22 C23 C24 C27 11.8(11) . . . . ?
C27 C24 C25 C26 0.1(9) . . . . ?
C23 C24 C25 C26 -179.0(6) . . . . ?
C24 C25 C26 C29 0.8(10) . . . . ?
C25 C24 C27 C28 0.1(9) . . . . ?
C23 C24 C27 C28 179.1(6) . . . . ?
C24 C27 C28 C29 -1.0(9) . . . . ?
C32 N3 C29 C26 13.2(9) . . . . ?
C30 N3 C29 C26 -173.4(6) . . . . ?
C32 N3 C29 C28 -168.0(6) . . . . ?
C30 N3 C29 C28 5.5(9) . . . . ?
C25 C26 C29 N3 177.3(6) . . . . ?
C25 C26 C29 C28 -1.6(9) . . . . ?
C27 C28 C29 N3 -177.2(5) . . . . ?
C27 C28 C29 C26 1.7(9) . . . . ?
C29 N3 C30 C31 -85.2(7) . . . . ?
C32 N3 C30 C31 88.6(7) . . . . ?
C29 N3 C32 C33 -94.8(7) . . . . ?
C30 N3 C32 C33 91.4(7) . . . . ?

_refine_diff_density_max         0.068
_refine_diff_density_min         -0.096
_refine_diff_density_rms         0.021

_shelxl_version_number           2013-4



_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
####################################################################### 
# 
# 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_BPB_KCB-30
_database_code_depnum_ccdc_archive 'CCDC 1963360'
loop_
_audit_author_name
_audit_author_address
'Bamaprasad Bag'
;CSIR Institute of Minerals and Materials Chemistry Bhubaneswar
India
;
_audit_update_record             
;
2020-01-22 deposited with the CCDC.	2020-07-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2[(C37 H40 N5 O2). (H1.5 O1)]'
_chemical_formula_sum            'C74 H85 N10 O6'
_chemical_formula_weight         1210.51

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                   9.309(2)
_cell_length_b                   14.055(3)
_cell_length_c                   25.600(6)
_cell_angle_alpha                90
_cell_angle_beta                 95.731(5)
_cell_angle_gamma                90
_cell_volume                     3332.6(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5523
_cell_measurement_theta_min      2.59
_cell_measurement_theta_max      22.95

_exptl_crystal_description       block
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_F_000             1294
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    0.078
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            25247
_diffrn_reflns_av_unetI/netI     0.0500
_diffrn_reflns_av_R_equivalents  0.0693
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.599
_diffrn_reflns_theta_max         23.363
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.794
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.794
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.794
_reflns_number_total             4782
_reflns_number_gt                3531
_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 APEX2'
_computing_cell_refinement       'BRUKER SAINT'
_computing_data_reduction        'BRUKER SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'BRUKER SHELXTL'
_computing_publication_material  'ORTEP 3 and DIAMOND 3.0'

_refine_special_details          
;
# start Validation Reply Form
;
_vrf_THETM01_BPB_KCB-30          
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
RESPONSE: The single crystal structure has severe disorder in its 
lattice water (sovent) molecule. The full set of data was collected, 
however, the very high angle data were omitted as those were dominated 
by noise.
;
_vrf_PLAT245_BPB_KCB-30          
;
PROBLEM: U(iso) H1O3      Smaller than U(eq) O3W       by      0.243 Ang**2
RESPONSE: The structure contains an disordered water (solvent) molecule, 
where one of the H-atom, assigned from the electron density, was located 
to occupy the special position, which leads to deviation from generally 
expected U(iso) of H-atom to be greater than U(eq) of the O-atom to which 
it is attached. The U(eq) of O(w)-atom was found to be higher than the average 
in this case and the ellipsoid is elongated due to higher thermal motion.
;
_vrf_PLAT390_BPB_KCB-30          
;
PROBLEM: Deviating Methyl C37       X-C-H Bond Angle ....         99 Degree
RESPONSE: There exists large amount of disorder in the structure. The C- atoms 
of alkyl chain attached to the rigid framework are dynamically disordered 
being involved in disorder with high thermal motion leading to these alerts.
;
_vrf_PLAT391_BPB_KCB-30          
;
PROBLEM: Deviating Methyl C25       H-C-H Bond Angle ....         98 Degree
RESPONSE: There exists large amount of disorder in the structure. The C- atoms 
of alkyl chain attached to the rigid framework are dynamically disordered 
being involved in disorder with high thermal motion leading to these alerts.
;
_vrf_PLAT420_BPB_KCB-30          
;
PROBLEM: D-H Without Acceptor       O3W      --H2O3     .     Please Check 
RESPONSE: The H-atom of the water (solvent) molecule was observed to occupy 
the special position, leading to disorder in the lattice.
;
# end Validation Reply Form

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1255P)²+0.0377P] 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
_refine_ls_extinction_coef       0.0126(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4782
_refine_ls_number_parameters     544
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0579
_refine_ls_wR_factor_ref         0.1826
_refine_ls_wR_factor_gt          0.1623
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.002
_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
O1 O 0.51027(17) 0.06385(11) 0.35677(7) 0.0547(5) Uani 1 1 d . . . . .
O2 O 0.3061(2) 0.42857(13) 0.22028(7) 0.0670(6) Uani 1 1 d . . . . .
N1 N 0.0413(3) -0.07051(17) 0.32393(11) 0.0701(7) Uani 1 1 d . . . . .
N2 N 0.9935(3) 0.17006(17) 0.39937(10) 0.0609(7) Uani 1 1 d . . . . .
N3 N 0.38885(19) 0.30789(13) 0.27687(7) 0.0401(5) Uani 1 1 d . . . . .
N4 N 0.3438(2) 0.35452(13) 0.31927(8) 0.0448(5) Uani 1 1 d . . . . .
N5 N 0.2136(3) 0.54299(16) 0.53587(8) 0.0632(7) Uani 1 1 d . . . . .
C1 C 0.2055(3) 0.13115(17) 0.26213(10) 0.0445(6) Uani 1 1 d . . . . .
C2 C 0.1024(2) 0.06516(17) 0.27259(10) 0.0463(6) Uani 1 1 d . . . . .
C3 C 0.1418(3) -0.00346(17) 0.31183(10) 0.0501(7) Uani 1 1 d . . . . .
C4 C 0.2797(3) -0.00167(18) 0.33792(11) 0.0526(7) Uani 1 1 d . . . . .
C5 C 0.7104(2) 0.25899(17) 0.30223(10) 0.0448(6) Uani 1 1 d . . . . .
C6 C 0.8431(3) 0.25057(17) 0.33046(10) 0.0466(6) Uani 1 1 d . . . . .
C7 C 0.8619(2) 0.17776(17) 0.36864(10) 0.0481(6) Uani 1 1 d . . . . .
C8 C 0.7478(3) 0.11619(18) 0.37584(10) 0.0484(6) Uani 1 1 d . . . . .
C9 C 0.3445(2) 0.13524(15) 0.28842(9) 0.0401(6) Uani 1 1 d . . . . .
C10 C 0.3785(2) 0.06711(16) 0.32637(10) 0.0456(6) Uani 1 1 d . . . . .
C11 C 0.5939(2) 0.19924(15) 0.30895(9) 0.0402(6) Uani 1 1 d . . . . .
C12 C 0.6162(2) 0.12784(16) 0.34586(9) 0.0427(6) Uani 1 1 d . . . . .
C13 C 0.4524(2) 0.20969(15) 0.27476(9) 0.0388(6) Uani 1 1 d . . . . .
C14 C 0.4783(2) 0.20736(15) 0.21692(9) 0.0405(6) Uani 1 1 d . . . . .
C15 C 0.5479(3) 0.13752(18) 0.19083(11) 0.0508(7) Uani 1 1 d . . . . .
C16 C 0.5652(3) 0.1536(2) 0.13850(12) 0.0622(8) Uani 1 1 d . . . . .
C17 C 0.5156(3) 0.2359(2) 0.11301(12) 0.0632(8) Uani 1 1 d . . . . .
C18 C 0.4466(3) 0.3051(2) 0.13918(11) 0.0548(7) Uani 1 1 d . . . . .
C19 C 0.4293(2) 0.28906(16) 0.19149(9) 0.0434(6) Uani 1 1 d . . . . .
C20 C 0.3666(3) 0.35237(17) 0.22900(10) 0.0463(6) Uani 1 1 d . . . . .
C21 C 0.0774(4) -0.1488(2) 0.36101(18) 0.1053(13) Uani 1 1 d . . . . .
H21A H 0.1475 -0.1898 0.3466 0.126 Uiso 1 1 calc R U . . .
H21B H 0.1228 -0.1222 0.3935 0.126 Uiso 1 1 calc R U . . .
C22 C -0.0429(5) -0.2057(3) 0.3727(2) 0.1405(19) Uani 1 1 d . . . . .
H22A H -0.0100 -0.2550 0.3970 0.211 Uiso 1 1 calc R U . . .
H22B H -0.0875 -0.2338 0.3410 0.211 Uiso 1 1 calc R U . . .
H22C H -0.1118 -0.1664 0.3881 0.211 Uiso 1 1 calc R U . . .
C23 C 1.0238(3) 0.0963(2) 0.43790(15) 0.0723(9) Uani 1 1 d . . . . .
C24 C 1.1672(4) 0.1122(3) 0.46852(17) 0.1146(14) Uani 1 1 d . . . . .
H24A H 1.1854 0.0622 0.4939 0.172 Uiso 1 1 calc R U . . .
H24B H 1.1667 0.1723 0.4863 0.172 Uiso 1 1 calc R U . . .
H24C H 1.2415 0.1122 0.4451 0.172 Uiso 1 1 calc R U . . .
C25 C -0.0454(3) 0.0661(3) 0.24332(14) 0.0594(8) Uani 1 1 d . . . . .
C26 C 0.9659(3) 0.3147(2) 0.32019(15) 0.0648(8) Uani 1 1 d . . . . .
C27 C 0.3664(3) 0.31944(18) 0.36557(10) 0.0441(6) Uani 1 1 d . . . . .
C28 C 0.3198(2) 0.37362(16) 0.40934(9) 0.0431(6) Uani 1 1 d . . . . .
C29 C 0.2314(3) 0.45291(17) 0.40174(11) 0.0437(6) Uani 1 1 d . . . . .
C30 C 0.1958(3) 0.50798(18) 0.44284(10) 0.0464(6) Uani 1 1 d . . . . .
C31 C 0.3664(3) 0.35056(19) 0.46095(10) 0.0555(7) Uani 1 1 d . . . . .
C32 C 0.3326(3) 0.4050(2) 0.50260(11) 0.0585(8) Uani 1 1 d . . . . .
C33 C 0.2466(3) 0.48652(17) 0.49466(9) 0.0489(7) Uani 1 1 d . . . . .
C34 C 0.1262(4) 0.6274(2) 0.52621(13) 0.0626(8) Uani 1 1 d . . . . .
C35 C 0.2097(5) 0.7110(3) 0.50848(18) 0.0843(11) Uani 1 1 d . . . . .
C36 C 0.2872(4) 0.5307(3) 0.58883(12) 0.0691(9) Uani 1 1 d . . . . .
C37 C 0.2093(5) 0.4634(4) 0.62139(18) 0.0926(12) Uani 1 1 d . . . . .
O3W O 1.4574(6) -0.0687(4) 0.4915(3) 0.246(3) Uani 1 1 d D . . . .
H35B H 0.276(5) 0.740(3) 0.5376(18) 0.127(15) Uiso 1 1 d . . . . .
H30 H 0.132(3) 0.5597(18) 0.4347(9) 0.053(7) Uiso 1 1 d . . . . .
H34A H 0.041(3) 0.6095(19) 0.5009(11) 0.069(9) Uiso 1 1 d . . . . .
H34B H 0.085(3) 0.640(2) 0.5566(13) 0.077(9) Uiso 1 1 d . . . . .
H8 H 0.757(3) 0.0596(19) 0.4011(10) 0.061(7) Uiso 1 1 d . . . . .
H4 H 0.313(3) -0.0472(18) 0.3660(10) 0.056(7) Uiso 1 1 d . . . . .
H31 H 0.419(3) 0.2935(19) 0.4668(10) 0.063(8) Uiso 1 1 d . . . . .
H27 H 0.421(3) 0.2581(18) 0.3730(9) 0.050(7) Uiso 1 1 d . . . . .
H15 H 0.585(3) 0.0768(19) 0.2072(10) 0.060(7) Uiso 1 1 d . . . . .
H29 H 0.199(3) 0.4716(16) 0.3689(10) 0.046(7) Uiso 1 1 d . . . . .
H18 H 0.414(3) 0.3680(18) 0.1227(9) 0.054(7) Uiso 1 1 d . . . . .
H5 H 0.700(3) 0.3095(18) 0.2750(10) 0.053(7) Uiso 1 1 d . . . . .
H32 H 0.367(3) 0.3859(18) 0.5356(11) 0.057(7) Uiso 1 1 d . . . . .
H17 H 0.528(3) 0.2449(19) 0.0753(12) 0.069(8) Uiso 1 1 d . . . . .
H1 H 0.180(2) 0.1805(16) 0.2333(9) 0.046(6) Uiso 1 1 d . . . . .
H25C H -0.072(3) 0.001(2) 0.2273(12) 0.087(10) Uiso 1 1 d . . . . .
H26B H 1.002(4) 0.350(2) 0.3505(14) 0.097(11) Uiso 1 1 d . . . . .
H25B H -0.119(4) 0.069(2) 0.2680(13) 0.086(10) Uiso 1 1 d . . . . .
H35A H 0.137(5) 0.772(3) 0.5063(15) 0.130(14) Uiso 1 1 d . . . . .
H26C H 1.053(4) 0.277(2) 0.3044(13) 0.102(11) Uiso 1 1 d . . . . .
H35C H 0.254(4) 0.700(2) 0.4759(15) 0.095(11) Uiso 1 1 d . . . . .
H2N2 H 1.069(4) 0.197(2) 0.3865(13) 0.093(12) Uiso 1 1 d . . . . .
H25A H -0.054(3) 0.110(2) 0.2211(12) 0.073(11) Uiso 1 1 d . . . . .
H26A H 0.936(4) 0.364(3) 0.2924(13) 0.096(11) Uiso 1 1 d . . . . .
H1N1 H -0.043(4) -0.064(2) 0.3082(13) 0.082(11) Uiso 1 1 d . . . . .
H23A H 0.946(3) 0.0928(19) 0.4662(12) 0.073(9) Uiso 1 1 d . . . . .
H37A H 0.200(5) 0.403(3) 0.6037(17) 0.129(17) Uiso 1 1 d . . . . .
H23B H 1.020(3) 0.036(2) 0.4227(12) 0.085(11) Uiso 1 1 d . . . . .
H16 H 0.609(3) 0.105(2) 0.1195(11) 0.075(8) Uiso 1 1 d . . . . .
H36A H 0.389(3) 0.5098(19) 0.5885(11) 0.070(8) Uiso 1 1 d . . . . .
H37C H 0.104(4) 0.478(2) 0.6269(14) 0.109(12) Uiso 1 1 d . . . . .
H36B H 0.291(3) 0.589(2) 0.6077(12) 0.083(10) Uiso 1 1 d . . . . .
H37B H 0.269(5) 0.476(3) 0.6591(19) 0.136(15) Uiso 1 1 d . . . . .
H1O3 H 1.5000 0.0000 0.5000 0.003(6) Uiso 1 2 d DS . P . .
H2O3 H 1.373(2) -0.045(5) 0.492(13) 1.0(3) Uiso 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C12 1.383(3) . ?
O1 C10 1.386(3) . ?
O2 C20 1.220(3) . ?
N1 C3 1.385(3) . ?
N1 C21 1.470(4) . ?
N1 H1N1 0.85(3) . ?
N2 C7 1.392(3) . ?
N2 C23 1.439(4) . ?
N2 H2N2 0.89(4) . ?
N3 N4 1.369(3) . ?
N3 C20 1.373(3) . ?
N3 C13 1.505(3) . ?
N4 C27 1.282(3) . ?
N5 C33 1.379(3) . ?
N5 C34 1.446(4) . ?
N5 C36 1.467(4) . ?
C1 C2 1.380(3) . ?
C1 C9 1.399(3) . ?
C1 H1 1.02(2) . ?
C2 C3 1.414(4) . ?
C2 C25 1.499(4) . ?
C3 C4 1.387(4) . ?
C4 C10 1.386(3) . ?
C4 H4 0.99(3) . ?
C5 C6 1.373(3) . ?
C5 C11 1.396(3) . ?
C5 H5 0.99(3) . ?
C6 C7 1.414(4) . ?
C6 C26 1.499(4) . ?
C7 C8 1.397(3) . ?
C8 C12 1.389(3) . ?
C8 H8 1.02(3) . ?
C9 C10 1.378(3) . ?
C9 C13 1.515(3) . ?
C11 C12 1.380(3) . ?
C11 C13 1.514(3) . ?
C13 C14 1.524(3) . ?
C14 C19 1.375(3) . ?
C14 C15 1.384(3) . ?
C15 C16 1.384(4) . ?
C15 H15 1.00(3) . ?
C16 C17 1.385(4) . ?
C16 H16 0.96(3) . ?
C17 C18 1.376(4) . ?
C17 H17 0.99(3) . ?
C18 C19 1.383(4) . ?
C18 H18 1.01(3) . ?
C19 C20 1.472(3) . ?
C21 C22 1.432(5) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 C24 1.496(5) . ?
C23 H23A 1.08(3) . ?
C23 H23B 0.93(3) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25C 1.02(3) . ?
C25 H25B 0.98(4) . ?
C25 H25A 0.84(3) . ?
C26 H26B 0.95(4) . ?
C26 H26C 1.08(4) . ?
C26 H26A 1.01(4) . ?
C27 C28 1.456(3) . ?
C27 H27 1.01(2) . ?
C28 C31 1.387(3) . ?
C28 C29 1.387(3) . ?
C29 C30 1.373(3) . ?
C29 H29 0.90(3) . ?
C30 C33 1.396(3) . ?
C30 H30 0.95(3) . ?
C31 C32 1.374(4) . ?
C31 H31 0.94(3) . ?
C32 C33 1.401(4) . ?
C32 H32 0.91(3) . ?
C34 C35 1.504(5) . ?
C34 H34A 1.01(3) . ?
C34 H34B 0.92(3) . ?
C35 H35B 1.00(5) . ?
C35 H35A 1.09(4) . ?
C35 H35C 0.98(4) . ?
C36 C37 1.496(5) . ?
C36 H36A 0.99(3) . ?
C36 H36B 0.96(3) . ?
C37 H37A 0.96(4) . ?
C37 H37C 1.03(4) . ?
C37 H37B 1.08(5) . ?
O3W H1O3 1.059(6) . ?
O3W H2O3 0.86(2) . ?

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
C12 O1 C10 118.27(18) . . ?
C3 N1 C21 122.6(3) . . ?
C3 N1 H1N1 115(2) . . ?
C21 N1 H1N1 122(2) . . ?
C7 N2 C23 123.0(2) . . ?
C7 N2 H2N2 116(2) . . ?
C23 N2 H2N2 117(2) . . ?
N4 N3 C20 117.30(18) . . ?
N4 N3 C13 128.33(18) . . ?
C20 N3 C13 114.24(18) . . ?
C27 N4 N3 120.9(2) . . ?
C33 N5 C34 120.4(2) . . ?
C33 N5 C36 121.3(2) . . ?
C34 N5 C36 117.2(2) . . ?
C2 C1 C9 124.2(2) . . ?
C2 C1 H1 118.8(13) . . ?
C9 C1 H1 117.0(13) . . ?
C1 C2 C3 117.4(2) . . ?
C1 C2 C25 121.2(3) . . ?
C3 C2 C25 121.4(2) . . ?
N1 C3 C4 121.2(3) . . ?
N1 C3 C2 119.3(2) . . ?
C4 C3 C2 119.5(2) . . ?
C3 C4 C10 120.8(2) . . ?
C3 C4 H4 123.2(14) . . ?
C10 C4 H4 116.0(15) . . ?
C6 C5 C11 123.6(2) . . ?
C6 C5 H5 116.7(14) . . ?
C11 C5 H5 119.7(14) . . ?
C5 C6 C7 118.0(2) . . ?
C5 C6 C26 121.2(3) . . ?
C7 C6 C26 120.8(2) . . ?
N2 C7 C8 121.0(2) . . ?
N2 C7 C6 119.2(2) . . ?
C8 C7 C6 119.8(2) . . ?
C12 C8 C7 119.7(2) . . ?
C12 C8 H8 117.3(15) . . ?
C7 C8 H8 123.0(14) . . ?
C10 C9 C1 116.5(2) . . ?
C10 C9 C13 122.1(2) . . ?
C1 C9 C13 121.3(2) . . ?
C9 C10 O1 123.1(2) . . ?
C9 C10 C4 121.6(2) . . ?
O1 C10 C4 115.2(2) . . ?
C12 C11 C5 117.1(2) . . ?
C12 C11 C13 122.0(2) . . ?
C5 C11 C13 120.8(2) . . ?
C11 C12 O1 123.3(2) . . ?
C11 C12 C8 121.9(2) . . ?
O1 C12 C8 114.8(2) . . ?
N3 C13 C11 113.00(17) . . ?
N3 C13 C9 110.67(17) . . ?
C11 C13 C9 110.97(18) . . ?
N3 C13 C14 98.95(17) . . ?
C11 C13 C14 110.29(18) . . ?
C9 C13 C14 112.47(18) . . ?
C19 C14 C15 120.9(2) . . ?
C19 C14 C13 111.39(19) . . ?
C15 C14 C13 127.7(2) . . ?
C16 C15 C14 117.2(3) . . ?
C16 C15 H15 118.6(15) . . ?
C14 C15 H15 124.2(15) . . ?
C15 C16 C17 121.8(3) . . ?
C15 C16 H16 118.2(17) . . ?
C17 C16 H16 120.0(17) . . ?
C18 C17 C16 120.8(3) . . ?
C18 C17 H17 119.2(16) . . ?
C16 C17 H17 120.0(16) . . ?
C17 C18 C19 117.5(3) . . ?
C17 C18 H18 123.2(14) . . ?
C19 C18 H18 119.3(14) . . ?
C14 C19 C18 122.0(2) . . ?
C14 C19 C20 109.3(2) . . ?
C18 C19 C20 128.7(2) . . ?
O2 C20 N3 126.1(2) . . ?
O2 C20 C19 128.1(2) . . ?
N3 C20 C19 105.82(19) . . ?
C22 C21 N1 114.9(3) . . ?
C22 C21 H21A 108.5 . . ?
N1 C21 H21A 108.5 . . ?
C22 C21 H21B 108.5 . . ?
N1 C21 H21B 108.5 . . ?
H21A C21 H21B 107.5 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N2 C23 C24 110.8(3) . . ?
N2 C23 H23A 113.3(15) . . ?
C24 C23 H23A 106.2(16) . . ?
N2 C23 H23B 112(2) . . ?
C24 C23 H23B 110(2) . . ?
H23A C23 H23B 104(3) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C2 C25 H25C 111.7(18) . . ?
C2 C25 H25B 110.1(19) . . ?
H25C C25 H25B 98(3) . . ?
C2 C25 H25A 111(2) . . ?
H25C C25 H25A 113(3) . . ?
H25B C25 H25A 113(3) . . ?
C6 C26 H26B 113(2) . . ?
C6 C26 H26C 112.5(18) . . ?
H26B C26 H26C 110(3) . . ?
C6 C26 H26A 112.2(19) . . ?
H26B C26 H26A 105(3) . . ?
H26C C26 H26A 104(3) . . ?
N4 C27 C28 118.4(2) . . ?
N4 C27 H27 122.6(13) . . ?
C28 C27 H27 118.9(13) . . ?
C31 C28 C29 116.5(2) . . ?
C31 C28 C27 121.4(2) . . ?
C29 C28 C27 122.0(2) . . ?
C30 C29 C28 122.0(3) . . ?
C30 C29 H29 117.8(15) . . ?
C28 C29 H29 120.1(15) . . ?
C29 C30 C33 121.4(2) . . ?
C29 C30 H30 117.3(15) . . ?
C33 C30 H30 121.2(15) . . ?
C32 C31 C28 122.3(3) . . ?
C32 C31 H31 120.3(17) . . ?
C28 C31 H31 117.3(17) . . ?
C31 C32 C33 121.0(3) . . ?
C31 C32 H32 117.9(16) . . ?
C33 C32 H32 121.2(16) . . ?
N5 C33 C30 121.5(2) . . ?
N5 C33 C32 121.8(2) . . ?
C30 C33 C32 116.7(2) . . ?
N5 C34 C35 113.2(3) . . ?
N5 C34 H34A 107.4(16) . . ?
C35 C34 H34A 113.5(16) . . ?
N5 C34 H34B 107.1(19) . . ?
C35 C34 H34B 111.8(18) . . ?
H34A C34 H34B 103(2) . . ?
C34 C35 H35B 113(2) . . ?
C34 C35 H35A 107(2) . . ?
H35B C35 H35A 93(3) . . ?
C34 C35 H35C 114(2) . . ?
H35B C35 H35C 115(3) . . ?
H35A C35 H35C 113(3) . . ?
N5 C36 C37 112.4(3) . . ?
N5 C36 H36A 112.6(16) . . ?
C37 C36 H36A 109.5(16) . . ?
N5 C36 H36B 110.8(19) . . ?
C37 C36 H36B 105.0(19) . . ?
H36A C36 H36B 106(3) . . ?
C36 C37 H37A 109(3) . . ?
C36 C37 H37C 119(2) . . ?
H37A C37 H37C 101(3) . . ?
C36 C37 H37B 99(2) . . ?
H37A C37 H37B 125(4) . . ?
H37C C37 H37B 105(3) . . ?
H1O3 O3W H2O3 88.0(15) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C20 N3 N4 C27 -177.0(2) . . . . ?
C13 N3 N4 C27 7.4(3) . . . . ?
C9 C1 C2 C3 -1.2(4) . . . . ?
C9 C1 C2 C25 179.0(2) . . . . ?
C21 N1 C3 C4 -6.0(4) . . . . ?
C21 N1 C3 C2 174.8(3) . . . . ?
C1 C2 C3 N1 179.4(2) . . . . ?
C25 C2 C3 N1 -0.8(4) . . . . ?
C1 C2 C3 C4 0.2(4) . . . . ?
C25 C2 C3 C4 -180.0(2) . . . . ?
N1 C3 C4 C10 -178.5(2) . . . . ?
C2 C3 C4 C10 0.7(4) . . . . ?
C11 C5 C6 C7 -0.5(4) . . . . ?
C11 C5 C6 C26 177.8(2) . . . . ?
C23 N2 C7 C8 3.6(4) . . . . ?
C23 N2 C7 C6 -177.8(3) . . . . ?
C5 C6 C7 N2 -177.3(2) . . . . ?
C26 C6 C7 N2 4.3(4) . . . . ?
C5 C6 C7 C8 1.2(3) . . . . ?
C26 C6 C7 C8 -177.1(2) . . . . ?
N2 C7 C8 C12 177.7(2) . . . . ?
C6 C7 C8 C12 -0.8(4) . . . . ?
C2 C1 C9 C10 1.2(3) . . . . ?
C2 C1 C9 C13 179.9(2) . . . . ?
C1 C9 C10 O1 -178.0(2) . . . . ?
C13 C9 C10 O1 3.3(4) . . . . ?
C1 C9 C10 C4 -0.2(4) . . . . ?
C13 C9 C10 C4 -178.9(2) . . . . ?
C12 O1 C10 C9 -4.8(3) . . . . ?
C12 O1 C10 C4 177.3(2) . . . . ?
C3 C4 C10 C9 -0.7(4) . . . . ?
C3 C4 C10 O1 177.2(2) . . . . ?
C6 C5 C11 C12 -0.6(3) . . . . ?
C6 C5 C11 C13 -177.2(2) . . . . ?
C5 C11 C12 O1 179.7(2) . . . . ?
C13 C11 C12 O1 -3.8(3) . . . . ?
C5 C11 C12 C8 1.0(3) . . . . ?
C13 C11 C12 C8 177.6(2) . . . . ?
C10 O1 C12 C11 5.0(3) . . . . ?
C10 O1 C12 C8 -176.2(2) . . . . ?
C7 C8 C12 C11 -0.3(4) . . . . ?
C7 C8 C12 O1 -179.1(2) . . . . ?
N4 N3 C13 C11 -62.2(3) . . . . ?
C20 N3 C13 C11 122.0(2) . . . . ?
N4 N3 C13 C9 62.9(3) . . . . ?
C20 N3 C13 C9 -112.8(2) . . . . ?
N4 N3 C13 C14 -178.84(19) . . . . ?
C20 N3 C13 C14 5.4(2) . . . . ?
C12 C11 C13 N3 126.9(2) . . . . ?
C5 C11 C13 N3 -56.7(3) . . . . ?
C12 C11 C13 C9 1.9(3) . . . . ?
C5 C11 C13 C9 178.31(19) . . . . ?
C12 C11 C13 C14 -123.4(2) . . . . ?
C5 C11 C13 C14 53.0(3) . . . . ?
C10 C9 C13 N3 -128.0(2) . . . . ?
C1 C9 C13 N3 53.4(3) . . . . ?
C10 C9 C13 C11 -1.7(3) . . . . ?
C1 C9 C13 C11 179.66(19) . . . . ?
C10 C9 C13 C14 122.4(2) . . . . ?
C1 C9 C13 C14 -56.3(3) . . . . ?
N3 C13 C14 C19 -2.8(2) . . . . ?
C11 C13 C14 C19 -121.5(2) . . . . ?
C9 C13 C14 C19 114.0(2) . . . . ?
N3 C13 C14 C15 173.9(2) . . . . ?
C11 C13 C14 C15 55.2(3) . . . . ?
C9 C13 C14 C15 -69.3(3) . . . . ?
C19 C14 C15 C16 -0.2(3) . . . . ?
C13 C14 C15 C16 -176.6(2) . . . . ?
C14 C15 C16 C17 0.2(4) . . . . ?
C15 C16 C17 C18 -0.1(4) . . . . ?
C16 C17 C18 C19 0.1(4) . . . . ?
C15 C14 C19 C18 0.2(3) . . . . ?
C13 C14 C19 C18 177.2(2) . . . . ?
C15 C14 C19 C20 -177.2(2) . . . . ?
C13 C14 C19 C20 -0.3(3) . . . . ?
C17 C18 C19 C14 -0.1(4) . . . . ?
C17 C18 C19 C20 176.8(2) . . . . ?
N4 N3 C20 O2 -2.4(4) . . . . ?
C13 N3 C20 O2 173.8(2) . . . . ?
N4 N3 C20 C19 177.92(17) . . . . ?
C13 N3 C20 C19 -5.8(2) . . . . ?
C14 C19 C20 O2 -176.0(2) . . . . ?
C18 C19 C20 O2 6.8(4) . . . . ?
C14 C19 C20 N3 3.6(3) . . . . ?
C18 C19 C20 N3 -173.6(2) . . . . ?
C3 N1 C21 C22 174.1(3) . . . . ?
C7 N2 C23 C24 -174.0(3) . . . . ?
N3 N4 C27 C28 178.21(18) . . . . ?
N4 C27 C28 C31 -166.4(2) . . . . ?
N4 C27 C28 C29 11.0(3) . . . . ?
C31 C28 C29 C30 2.3(3) . . . . ?
C27 C28 C29 C30 -175.3(2) . . . . ?
C28 C29 C30 C33 -0.3(4) . . . . ?
C29 C28 C31 C32 -2.6(4) . . . . ?
C27 C28 C31 C32 174.9(2) . . . . ?
C28 C31 C32 C33 1.0(4) . . . . ?
C34 N5 C33 C30 -0.8(4) . . . . ?
C36 N5 C33 C30 -168.8(3) . . . . ?
C34 N5 C33 C32 179.1(3) . . . . ?
C36 N5 C33 C32 11.1(4) . . . . ?
C29 C30 C33 N5 178.5(2) . . . . ?
C29 C30 C33 C32 -1.4(4) . . . . ?
C31 C32 C33 N5 -178.8(3) . . . . ?
C31 C32 C33 C30 1.1(4) . . . . ?
C33 N5 C34 C35 -79.7(4) . . . . ?
C36 N5 C34 C35 88.8(4) . . . . ?
C33 N5 C36 C37 -91.6(4) . . . . ?
C34 N5 C36 C37 100.1(4) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1N1 O2 0.85(3) 2.49(4) 3.319(4) 166(3) 2_545

_refine_diff_density_max         0.395
_refine_diff_density_min         -0.249
_refine_diff_density_rms         0.065

_shelxl_version_number           2013-4



_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
