# Supplementary Information (SI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2025

####################################################################### 
# 
# 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_bhrigu-1
_database_code_depnum_ccdc_archive 'CCDC 2423117'
loop_
_audit_author_name
_audit_author_address
'Malay Dolai'
;Prabhat Kumar College, West Bengal, India
India
;
_audit_update_record             
;
2025-02-11 deposited with the CCDC.	2025-07-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H30 N10 O2 Zn, 2(Cl O4), C H4 O, O'
_chemical_formula_sum            'C33 H34 Cl2 N10 O12 Zn'
_chemical_formula_weight         898.99

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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'

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

_cell_length_a                   12.1710(17)
_cell_length_b                   17.084(2)
_cell_length_c                   19.615(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.351(4)
_cell_angle_gamma                90.00
_cell_volume                     4045.0(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    250
_cell_measurement_theta_min      2.07
_cell_measurement_theta_max      27.18

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1848.0
_exptl_absorpt_coefficient_mu    0.811
_exptl_absorpt_correction_type   Empirical
_exptl_absorpt_correction_T_min  0.839
_exptl_absorpt_correction_T_max  0.922
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            147205
_diffrn_reflns_av_R_equivalents  0.0951
_diffrn_reflns_av_sigmaI/netI    0.0390
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.07
_diffrn_reflns_theta_max         27.18
_reflns_number_total             8985
_reflns_number_gt                6668
_reflns_threshold_expression     >2sigma(I)

_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  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8948
_refine_ls_number_parameters     529
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0976
_refine_ls_R_factor_gt           0.0731
_refine_ls_wR_factor_ref         0.2315
_refine_ls_wR_factor_gt          0.2207
_refine_ls_goodness_of_fit_ref   1.587
_refine_ls_restrained_S_all      1.587
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.48560(3) 0.69853(2) 0.13110(2) 0.03906(18) Uani 1 1 d . . .
O1 O 0.3265(2) 0.73618(18) 0.13941(15) 0.0538(7) Uani 1 1 d . . .
O1S O 0.4538(7) 0.1797(4) 0.1177(3) 0.147(2) Uani 1 1 d . . .
N9 N 0.1469(3) 0.7654(2) 0.1236(2) 0.0533(9) Uani 1 1 d . . .
N1 N 0.6167(3) 0.63011(18) 0.09739(17) 0.0429(7) Uani 1 1 d . . .
N2 N 0.4823(3) 0.6064(2) 0.00482(18) 0.0486(8) Uani 1 1 d . . .
H54 H 0.4622 0.5856 -0.0347 0.058 Uiso 1 1 calc R . .
N3 N 0.4068(2) 0.64350(17) 0.03902(16) 0.0389(7) Uani 1 1 d . . .
N4 N 0.5453(3) 0.78467(19) 0.20583(16) 0.0436(7) Uani 1 1 d . . .
O2 O 0.5227(3) 0.78493(16) 0.06101(15) 0.0510(7) Uani 1 1 d . . .
N6 N 0.5857(3) 0.89043(19) 0.01147(18) 0.0490(8) Uani 1 1 d . . .
N7 N 0.5384(3) 0.7591(2) 0.27161(18) 0.0561(9) Uani 1 1 d . . .
H7 H 0.5524 0.7903 0.3061 0.067 Uiso 1 1 calc R . .
N8 N 0.4798(3) 0.63962(18) 0.22583(17) 0.0434(7) Uani 1 1 d . . .
C1 C 0.7229(3) 0.6209(3) 0.1257(2) 0.0539(10) Uani 1 1 d . . .
C2 C 0.7537(4) 0.6500(4) 0.1982(3) 0.0858(18) Uani 1 1 d . . .
H1 H 0.7510 0.7061 0.1987 0.129 Uiso 1 1 calc R . .
H3 H 0.8273 0.6328 0.2151 0.129 Uiso 1 1 calc R . .
H53 H 0.7024 0.6295 0.2270 0.129 Uiso 1 1 calc R . .
C3 C 0.7987(4) 0.5867(3) 0.0884(3) 0.0647(12) Uani 1 1 d . . .
H4 H 0.8719 0.5802 0.1078 0.078 Uiso 1 1 calc R . .
C4 C 0.7653(3) 0.5626(3) 0.0229(3) 0.0558(11) Uani 1 1 d . . .
N11 N 0.6601(3) 0.5699(2) -0.0052(2) 0.0530(9) Uani 1 1 d . . .
H11 H 0.6380 0.5544 -0.0463 0.064 Uiso 1 1 calc R . .
C6 C 0.5908(3) 0.6025(2) 0.0341(2) 0.0422(8) Uani 1 1 d . . .
C7 C 0.3074(3) 0.6486(2) 0.0088(2) 0.0453(9) Uani 1 1 d . . .
H5 H 0.2911 0.6248 -0.0340 0.054 Uiso 1 1 calc R . .
C8 C 0.2188(3) 0.6890(2) 0.0370(2) 0.0421(9) Uani 1 1 d . . .
C9 C 0.2365(3) 0.7297(2) 0.1024(2) 0.0426(8) Uani 1 1 d . . .
C10 C 0.0416(3) 0.7665(3) 0.0862(3) 0.0548(10) Uani 1 1 d . . .
C11 C 0.0246(3) 0.7309(3) 0.0225(2) 0.0534(11) Uani 1 1 d . . .
C12 C -0.0819(4) 0.7343(3) -0.0160(3) 0.0717(14) Uani 1 1 d . . .
H9 H -0.0952 0.7110 -0.0591 0.086 Uiso 1 1 calc R . .
C13 C -0.1640(4) 0.7720(4) 0.0111(5) 0.101(2) Uani 1 1 d . . .
H8 H -0.2337 0.7752 -0.0144 0.121 Uiso 1 1 calc R . .
C14 C -0.1469(5) 0.8064(4) 0.0761(5) 0.101(2) Uani 1 1 d . . .
H52 H -0.2057 0.8306 0.0936 0.121 Uiso 1 1 calc R . .
C15 C -0.0447(5) 0.8050(3) 0.1142(4) 0.0787(16) Uani 1 1 d . . .
H6 H -0.0325 0.8286 0.1572 0.094 Uiso 1 1 calc R . .
C16 C 0.1166(3) 0.6909(2) -0.0009(2) 0.0480(9) Uani 1 1 d . . .
H10 H 0.1063 0.6655 -0.0432 0.058 Uiso 1 1 calc R . .
C17 C 0.8445(4) 0.5287(3) -0.0218(3) 0.0793(17) Uani 1 1 d . . .
H13 H 0.8140 0.4813 -0.0427 0.119 Uiso 1 1 calc R . .
H14 H 0.9137 0.5173 0.0057 0.119 Uiso 1 1 calc R . .
H12 H 0.8564 0.5656 -0.0570 0.119 Uiso 1 1 calc R . .
C18 C 0.5747(3) 0.8564(2) 0.1994(2) 0.0485(9) Uani 1 1 d . . .
H20 H 0.5868 0.8871 0.2388 0.058 Uiso 1 1 calc R . .
C19 C 0.5901(3) 0.8924(2) 0.1337(2) 0.0455(9) Uani 1 1 d . . .
C20 C 0.5642(3) 0.8519(2) 0.0691(2) 0.0429(9) Uani 1 1 d . . .
C21 C 0.6314(3) 0.9652(3) 0.0119(3) 0.0541(11) Uani 1 1 d . . .
C22 C 0.6528(4) 0.9999(3) -0.0497(3) 0.0687(13) Uani 1 1 d . . .
H19 H 0.6382 0.9728 -0.0910 0.082 Uiso 1 1 calc R . .
C23 C 0.6951(5) 1.0736(4) -0.0484(4) 0.0865(19) Uani 1 1 d . . .
H18 H 0.7062 1.0977 -0.0895 0.104 Uiso 1 1 calc R . .
C24 C 0.7215(6) 1.1129(4) 0.0117(4) 0.100(2) Uani 1 1 d . . .
H17 H 0.7533 1.1623 0.0113 0.120 Uiso 1 1 calc R . .
C25 C 0.7012(5) 1.0797(3) 0.0745(4) 0.0859(18) Uani 1 1 d . . .
H16 H 0.7183 1.1071 0.1154 0.103 Uiso 1 1 calc R . .
C26 C 0.6549(4) 1.0047(3) 0.0744(3) 0.0601(12) Uani 1 1 d . . .
C27 C 0.6336(4) 0.9651(3) 0.1353(3) 0.0573(11) Uani 1 1 d . . .
H15 H 0.6501 0.9902 0.1775 0.069 Uiso 1 1 calc R . .
C28 C 0.5088(3) 0.6826(2) 0.2811(2) 0.0461(9) Uani 1 1 d . . .
C29 C 0.4485(4) 0.5648(3) 0.2358(2) 0.0538(10) Uani 1 1 d . . .
C30 C 0.4513(5) 0.5381(3) 0.3023(3) 0.0690(13) Uani 1 1 d . . .
H25 H 0.4317 0.4866 0.3103 0.083 Uiso 1 1 calc R . .
C31 C 0.4824(4) 0.5867(3) 0.3562(2) 0.0672(13) Uani 1 1 d . . .
N10 N 0.5132(3) 0.6610(3) 0.3461(2) 0.0656(11) Uani 1 1 d . . .
H10A H 0.5342 0.6923 0.3796 0.079 Uiso 1 1 calc R . .
C33 C 0.4865(7) 0.5584(4) 0.4297(3) 0.105(2) Uani 1 1 d . . .
H23 H 0.4786 0.5025 0.4300 0.157 Uiso 1 1 calc R . .
H24 H 0.4272 0.5819 0.4504 0.157 Uiso 1 1 calc R . .
H22 H 0.5561 0.5728 0.4552 0.157 Uiso 1 1 calc R . .
C34 C 0.4111(5) 0.5173(3) 0.1746(3) 0.0737(14) Uani 1 1 d . . .
H27 H 0.3361 0.5309 0.1575 0.111 Uiso 1 1 calc R . .
H28 H 0.4149 0.4628 0.1867 0.111 Uiso 1 1 calc R . .
H26 H 0.4579 0.5272 0.1397 0.111 Uiso 1 1 calc R . .
O2S O 0.1959(6) 0.8540(4) 0.2440(3) 0.148(3) Uani 1 1 d . . .
H2S H 0.1327 0.8390 0.2307 0.222 Uiso 1 1 calc R . .
C1S C 0.2406(10) 0.8086(6) 0.2988(5) 0.157(4) Uani 1 1 d . . .
H1S1 H 0.3126 0.7905 0.2909 0.235 Uiso 1 1 calc R . .
H1S2 H 0.1933 0.7645 0.3034 0.235 Uiso 1 1 calc R . .
H1S3 H 0.2470 0.8392 0.3401 0.235 Uiso 1 1 calc R . .
Cl1 Cl 0.66309(16) 0.35872(13) 0.18187(9) 0.1049(6) Uani 1 1 d . . .
O2C O 0.6666(6) 0.3655(6) 0.2496(3) 0.182(3) Uani 1 1 d . . .
O1C O 0.5590(6) 0.3400(6) 0.1474(4) 0.212(4) Uani 1 1 d . . .
O4C O 0.7527(8) 0.3276(8) 0.1620(4) 0.304(8) Uani 1 1 d . . .
O3C O 0.6605(11) 0.4260(4) 0.1520(6) 0.258(6) Uani 1 1 d . . .
Cl2 Cl 0.0941(2) 0.5403(2) 0.22795(13) 0.1416(10) Uani 1 1 d . . .
O5C O 0.0025(6) 0.5577(6) 0.2549(5) 0.224(5) Uani 1 1 d . . .
O6C O 0.1098(10) 0.5709(6) 0.1675(5) 0.237(5) Uani 1 1 d . . .
O8C O 0.1556(8) 0.4887(7) 0.2664(5) 0.238(5) Uani 1 1 d . . .
O7C O 0.0389(11) 0.4724(8) 0.1836(6) 0.250(5) Uani 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
Zn1 O1 2.067(3) . ?
Zn1 O2 2.105(3) . ?
Zn1 N8 2.122(3) . ?
Zn1 N4 2.138(3) . ?
Zn1 N1 2.150(3) . ?
Zn1 N3 2.150(3) . ?
O1 C9 1.238(5) . ?
N9 C9 1.360(5) . ?
N9 C10 1.393(6) . ?
N1 C6 1.328(5) . ?
N1 C1 1.349(5) . ?
N2 N3 1.362(4) . ?
N2 C6 1.373(5) . ?
N2 H54 0.8600 . ?
N3 C7 1.280(5) . ?
N4 C18 1.288(5) . ?
N4 N7 1.375(4) . ?
O2 C20 1.253(5) . ?
N6 C20 1.362(5) . ?
N6 C21 1.392(5) . ?
N7 C28 1.375(5) . ?
N7 H7 0.8600 . ?
N8 C28 1.320(5) . ?
N8 C29 1.354(5) . ?
C1 C3 1.379(6) . ?
C1 C2 1.507(7) . ?
C2 H1 0.9600 . ?
C2 H3 0.9600 . ?
C2 H53 0.9600 . ?
C3 C4 1.361(7) . ?
C3 H4 0.9300 . ?
C4 N11 1.333(6) . ?
C4 C17 1.499(6) . ?
N11 C6 1.334(5) . ?
N11 H11 0.8600 . ?
C7 C8 1.449(5) . ?
C7 H5 0.9300 . ?
C8 C16 1.365(6) . ?
C8 C9 1.451(6) . ?
C10 C11 1.381(7) . ?
C10 C15 1.409(6) . ?
C11 C12 1.415(6) . ?
C11 C16 1.436(6) . ?
C12 C13 1.354(8) . ?
C12 H9 0.9300 . ?
C13 C14 1.394(10) . ?
C13 H8 0.9300 . ?
C14 C15 1.368(9) . ?
C14 H52 0.9300 . ?
C15 H6 0.9300 . ?
C16 H10 0.9300 . ?
C17 H13 0.9600 . ?
C17 H14 0.9600 . ?
C17 H12 0.9600 . ?
C18 C19 1.461(6) . ?
C18 H20 0.9300 . ?
C19 C27 1.349(6) . ?
C19 C20 1.443(6) . ?
C21 C26 1.395(7) . ?
C21 C22 1.400(6) . ?
C22 C23 1.360(8) . ?
C22 H19 0.9300 . ?
C23 C24 1.359(10) . ?
C23 H18 0.9300 . ?
C24 C25 1.406(9) . ?
C24 H17 0.9300 . ?
C25 C26 1.400(6) . ?
C25 H16 0.9300 . ?
C26 C27 1.426(7) . ?
C27 H15 0.9300 . ?
C28 N10 1.322(5) . ?
C29 C30 1.378(6) . ?
C29 C34 1.473(7) . ?
C30 C31 1.360(7) . ?
C30 H25 0.9300 . ?
C31 N10 1.345(6) . ?
C31 C33 1.516(7) . ?
N10 H10A 0.8600 . ?
C33 H23 0.9600 . ?
C33 H24 0.9600 . ?
C33 H22 0.9600 . ?
C34 H27 0.9600 . ?
C34 H28 0.9600 . ?
C34 H26 0.9600 . ?
O2S C1S 1.379(11) . ?
O2S H2S 0.8200 . ?
C1S H1S1 0.9600 . ?
C1S H1S2 0.9600 . ?
C1S H1S3 0.9600 . ?
Cl1 O3C 1.288(8) . ?
Cl1 O4C 1.316(7) . ?
Cl1 O2C 1.329(6) . ?
Cl1 O1C 1.395(7) . ?
Cl2 O5C 1.327(6) . ?
Cl2 O8C 1.328(7) . ?
Cl2 O6C 1.333(7) . ?
Cl2 O7C 1.550(14) . ?

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
O1 Zn1 O2 96.60(12) . . ?
O1 Zn1 N8 86.69(12) . . ?
O2 Zn1 N8 159.75(12) . . ?
O1 Zn1 N4 88.37(12) . . ?
O2 Zn1 N4 83.26(12) . . ?
N8 Zn1 N4 76.85(12) . . ?
O1 Zn1 N1 158.99(12) . . ?
O2 Zn1 N1 87.16(12) . . ?
N8 Zn1 N1 96.92(12) . . ?
N4 Zn1 N1 112.62(13) . . ?
O1 Zn1 N3 83.13(11) . . ?
O2 Zn1 N3 82.41(11) . . ?
N8 Zn1 N3 117.84(12) . . ?
N4 Zn1 N3 162.36(12) . . ?
N1 Zn1 N3 76.88(12) . . ?
C9 O1 Zn1 133.9(3) . . ?
C9 N9 C10 124.4(4) . . ?
C6 N1 C1 116.4(3) . . ?
C6 N1 Zn1 112.6(2) . . ?
C1 N1 Zn1 130.3(3) . . ?
N3 N2 C6 119.4(3) . . ?
N3 N2 H54 120.3 . . ?
C6 N2 H54 120.3 . . ?
C7 N3 N2 117.4(3) . . ?
C7 N3 Zn1 130.8(3) . . ?
N2 N3 Zn1 111.1(2) . . ?
C18 N4 N7 116.4(3) . . ?
C18 N4 Zn1 131.5(3) . . ?
N7 N4 Zn1 111.7(2) . . ?
C20 O2 Zn1 132.4(3) . . ?
C20 N6 C21 123.8(4) . . ?
C28 N7 N4 118.5(3) . . ?
C28 N7 H7 120.7 . . ?
N4 N7 H7 120.7 . . ?
C28 N8 C29 117.2(3) . . ?
C28 N8 Zn1 114.8(3) . . ?
C29 N8 Zn1 128.0(3) . . ?
N1 C1 C3 120.1(4) . . ?
N1 C1 C2 117.3(4) . . ?
C3 C1 C2 122.6(4) . . ?
C1 C2 H1 109.5 . . ?
C1 C2 H3 109.5 . . ?
H1 C2 H3 109.5 . . ?
C1 C2 H53 109.5 . . ?
H1 C2 H53 109.5 . . ?
H3 C2 H53 109.5 . . ?
C4 C3 C1 119.4(4) . . ?
C4 C3 H4 120.3 . . ?
C1 C3 H4 120.3 . . ?
N11 C4 C3 121.1(4) . . ?
N11 C4 C17 116.8(5) . . ?
C3 C4 C17 122.2(4) . . ?
C4 N11 C6 116.4(4) . . ?
C4 N11 H11 121.8 . . ?
C6 N11 H11 121.8 . . ?
N1 C6 N11 126.6(4) . . ?
N1 C6 N2 118.3(3) . . ?
N11 C6 N2 115.1(4) . . ?
N3 C7 C8 124.1(4) . . ?
N3 C7 H5 117.9 . . ?
C8 C7 H5 117.9 . . ?
C16 C8 C7 118.3(4) . . ?
C16 C8 C9 119.5(4) . . ?
C7 C8 C9 122.2(3) . . ?
O1 C9 N9 117.7(4) . . ?
O1 C9 C8 125.6(3) . . ?
N9 C9 C8 116.8(4) . . ?
C11 C10 N9 119.4(4) . . ?
C11 C10 C15 121.8(5) . . ?
N9 C10 C15 118.8(5) . . ?
C10 C11 C12 119.0(4) . . ?
C10 C11 C16 117.8(4) . . ?
C12 C11 C16 123.2(5) . . ?
C13 C12 C11 118.8(6) . . ?
C13 C12 H9 120.6 . . ?
C11 C12 H9 120.6 . . ?
C12 C13 C14 121.9(6) . . ?
C12 C13 H8 119.0 . . ?
C14 C13 H8 119.0 . . ?
C15 C14 C13 120.7(5) . . ?
C15 C14 H52 119.6 . . ?
C13 C14 H52 119.6 . . ?
C14 C15 C10 117.8(6) . . ?
C14 C15 H6 121.1 . . ?
C10 C15 H6 121.1 . . ?
C8 C16 C11 122.1(4) . . ?
C8 C16 H10 119.0 . . ?
C11 C16 H10 119.0 . . ?
C4 C17 H13 109.5 . . ?
C4 C17 H14 109.5 . . ?
H13 C17 H14 109.5 . . ?
C4 C17 H12 109.5 . . ?
H13 C17 H12 109.5 . . ?
H14 C17 H12 109.5 . . ?
N4 C18 C19 123.7(4) . . ?
N4 C18 H20 118.1 . . ?
C19 C18 H20 118.1 . . ?
C27 C19 C20 120.2(4) . . ?
C27 C19 C18 117.5(4) . . ?
C20 C19 C18 122.3(3) . . ?
O2 C20 N6 117.0(4) . . ?
O2 C20 C19 126.0(3) . . ?
N6 C20 C19 117.0(3) . . ?
N6 C21 C26 119.0(4) . . ?
N6 C21 C22 120.0(5) . . ?
C26 C21 C22 120.9(4) . . ?
C23 C22 C21 119.2(6) . . ?
C23 C22 H19 120.4 . . ?
C21 C22 H19 120.4 . . ?
C24 C23 C22 121.3(6) . . ?
C24 C23 H18 119.3 . . ?
C22 C23 H18 119.3 . . ?
C23 C24 C25 120.9(5) . . ?
C23 C24 H17 119.6 . . ?
C25 C24 H17 119.6 . . ?
C26 C25 C24 118.9(6) . . ?
C26 C25 H16 120.5 . . ?
C24 C25 H16 120.5 . . ?
C21 C26 C25 118.7(5) . . ?
C21 C26 C27 118.0(4) . . ?
C25 C26 C27 123.3(5) . . ?
C19 C27 C26 122.0(5) . . ?
C19 C27 H15 119.0 . . ?
C26 C27 H15 119.0 . . ?
N8 C28 N10 127.6(4) . . ?
N8 C28 N7 117.7(3) . . ?
N10 C28 N7 114.7(4) . . ?
N8 C29 C30 118.5(4) . . ?
N8 C29 C34 117.8(4) . . ?
C30 C29 C34 123.8(4) . . ?
C31 C30 C29 120.2(4) . . ?
C31 C30 H25 119.9 . . ?
C29 C30 H25 119.9 . . ?
N10 C31 C30 121.2(4) . . ?
N10 C31 C33 117.7(5) . . ?
C30 C31 C33 121.1(5) . . ?
C28 N10 C31 115.3(4) . . ?
C28 N10 H10A 122.3 . . ?
C31 N10 H10A 122.3 . . ?
C31 C33 H23 109.5 . . ?
C31 C33 H24 109.5 . . ?
H23 C33 H24 109.5 . . ?
C31 C33 H22 109.5 . . ?
H23 C33 H22 109.5 . . ?
H24 C33 H22 109.5 . . ?
C29 C34 H27 109.5 . . ?
C29 C34 H28 109.5 . . ?
H27 C34 H28 109.5 . . ?
C29 C34 H26 109.5 . . ?
H27 C34 H26 109.5 . . ?
H28 C34 H26 109.5 . . ?
C1S O2S H2S 109.5 . . ?
O2S C1S H1S1 109.5 . . ?
O2S C1S H1S2 109.5 . . ?
H1S1 C1S H1S2 109.5 . . ?
O2S C1S H1S3 109.5 . . ?
H1S1 C1S H1S3 109.5 . . ?
H1S2 C1S H1S3 109.5 . . ?
O3C Cl1 O4C 101.5(8) . . ?
O3C Cl1 O2C 111.9(6) . . ?
O4C Cl1 O2C 114.2(5) . . ?
O3C Cl1 O1C 90.9(8) . . ?
O4C Cl1 O1C 119.9(6) . . ?
O2C Cl1 O1C 114.6(5) . . ?
O5C Cl2 O8C 111.3(6) . . ?
O5C Cl2 O6C 119.4(6) . . ?
O8C Cl2 O6C 129.1(6) . . ?
O5C Cl2 O7C 93.8(7) . . ?
O8C Cl2 O7C 89.6(7) . . ?
O6C Cl2 O7C 84.0(6) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 Zn1 O1 C9 77.7(4) . . . . ?
N8 Zn1 O1 C9 -122.4(4) . . . . ?
N4 Zn1 O1 C9 160.7(4) . . . . ?
N1 Zn1 O1 C9 -21.6(6) . . . . ?
N3 Zn1 O1 C9 -3.8(4) . . . . ?
O1 Zn1 N1 C6 29.8(5) . . . . ?
O2 Zn1 N1 C6 -71.2(3) . . . . ?
N8 Zn1 N1 C6 128.7(3) . . . . ?
N4 Zn1 N1 C6 -152.7(2) . . . . ?
N3 Zn1 N1 C6 11.6(2) . . . . ?
O1 Zn1 N1 C1 -160.7(4) . . . . ?
O2 Zn1 N1 C1 98.2(4) . . . . ?
N8 Zn1 N1 C1 -61.9(4) . . . . ?
N4 Zn1 N1 C1 16.7(4) . . . . ?
N3 Zn1 N1 C1 -178.9(4) . . . . ?
C6 N2 N3 C7 177.3(3) . . . . ?
C6 N2 N3 Zn1 5.6(4) . . . . ?
O1 Zn1 N3 C7 7.2(3) . . . . ?
O2 Zn1 N3 C7 -90.4(3) . . . . ?
N8 Zn1 N3 C7 89.8(4) . . . . ?
N4 Zn1 N3 C7 -54.5(6) . . . . ?
N1 Zn1 N3 C7 -179.2(4) . . . . ?
O1 Zn1 N3 N2 177.5(3) . . . . ?
O2 Zn1 N3 N2 79.9(2) . . . . ?
N8 Zn1 N3 N2 -99.9(2) . . . . ?
N4 Zn1 N3 N2 115.8(4) . . . . ?
N1 Zn1 N3 N2 -9.0(2) . . . . ?
O1 Zn1 N4 C18 -90.4(4) . . . . ?
O2 Zn1 N4 C18 6.5(4) . . . . ?
N8 Zn1 N4 C18 -177.4(4) . . . . ?
N1 Zn1 N4 C18 90.5(4) . . . . ?
N3 Zn1 N4 C18 -29.4(7) . . . . ?
O1 Zn1 N4 N7 81.7(3) . . . . ?
O2 Zn1 N4 N7 178.5(3) . . . . ?
N8 Zn1 N4 N7 -5.3(3) . . . . ?
N1 Zn1 N4 N7 -97.4(3) . . . . ?
N3 Zn1 N4 N7 142.7(4) . . . . ?
O1 Zn1 O2 C20 89.6(4) . . . . ?
N8 Zn1 O2 C20 -8.8(6) . . . . ?
N4 Zn1 O2 C20 2.0(4) . . . . ?
N1 Zn1 O2 C20 -111.1(4) . . . . ?
N3 Zn1 O2 C20 171.7(4) . . . . ?
C18 N4 N7 C28 -179.2(4) . . . . ?
Zn1 N4 N7 C28 7.5(5) . . . . ?
O1 Zn1 N8 C28 -86.2(3) . . . . ?
O2 Zn1 N8 C28 13.9(5) . . . . ?
N4 Zn1 N8 C28 2.9(3) . . . . ?
N1 Zn1 N8 C28 114.6(3) . . . . ?
N3 Zn1 N8 C28 -166.7(3) . . . . ?
O1 Zn1 N8 C29 92.5(3) . . . . ?
O2 Zn1 N8 C29 -167.4(3) . . . . ?
N4 Zn1 N8 C29 -178.4(4) . . . . ?
N1 Zn1 N8 C29 -66.8(4) . . . . ?
N3 Zn1 N8 C29 12.0(4) . . . . ?
C6 N1 C1 C3 2.1(6) . . . . ?
Zn1 N1 C1 C3 -167.0(3) . . . . ?
C6 N1 C1 C2 -178.5(4) . . . . ?
Zn1 N1 C1 C2 12.4(6) . . . . ?
N1 C1 C3 C4 0.1(7) . . . . ?
C2 C1 C3 C4 -179.2(5) . . . . ?
C1 C3 C4 N11 -1.6(7) . . . . ?
C1 C3 C4 C17 176.9(5) . . . . ?
C3 C4 N11 C6 0.7(6) . . . . ?
C17 C4 N11 C6 -177.9(4) . . . . ?
C1 N1 C6 N11 -3.3(6) . . . . ?
Zn1 N1 C6 N11 167.7(3) . . . . ?
C1 N1 C6 N2 176.2(4) . . . . ?
Zn1 N1 C6 N2 -12.8(4) . . . . ?
C4 N11 C6 N1 1.9(6) . . . . ?
C4 N11 C6 N2 -177.6(4) . . . . ?
N3 N2 C6 N1 4.9(5) . . . . ?
N3 N2 C6 N11 -175.5(3) . . . . ?
N2 N3 C7 C8 -177.3(3) . . . . ?
Zn1 N3 C7 C8 -7.5(6) . . . . ?
N3 C7 C8 C16 179.2(4) . . . . ?
N3 C7 C8 C9 1.8(6) . . . . ?
Zn1 O1 C9 N9 -177.6(3) . . . . ?
Zn1 O1 C9 C8 0.6(6) . . . . ?
C10 N9 C9 O1 177.0(4) . . . . ?
C10 N9 C9 C8 -1.4(6) . . . . ?
C16 C8 C9 O1 -175.5(4) . . . . ?
C7 C8 C9 O1 1.9(6) . . . . ?
C16 C8 C9 N9 2.7(5) . . . . ?
C7 C8 C9 N9 -179.9(4) . . . . ?
C9 N9 C10 C11 -1.5(7) . . . . ?
C9 N9 C10 C15 179.5(4) . . . . ?
N9 C10 C11 C12 -178.2(4) . . . . ?
C15 C10 C11 C12 0.9(7) . . . . ?
N9 C10 C11 C16 2.9(6) . . . . ?
C15 C10 C11 C16 -178.0(4) . . . . ?
C10 C11 C12 C13 -0.3(8) . . . . ?
C16 C11 C12 C13 178.6(5) . . . . ?
C11 C12 C13 C14 -1.1(10) . . . . ?
C12 C13 C14 C15 1.8(11) . . . . ?
C13 C14 C15 C10 -1.2(10) . . . . ?
C11 C10 C15 C14 -0.2(8) . . . . ?
N9 C10 C15 C14 178.9(5) . . . . ?
C7 C8 C16 C11 -178.8(4) . . . . ?
C9 C8 C16 C11 -1.2(6) . . . . ?
C10 C11 C16 C8 -1.6(6) . . . . ?
C12 C11 C16 C8 179.5(4) . . . . ?
N7 N4 C18 C19 177.7(4) . . . . ?
Zn1 N4 C18 C19 -10.6(6) . . . . ?
N4 C18 C19 C27 -172.3(4) . . . . ?
N4 C18 C19 C20 5.4(6) . . . . ?
Zn1 O2 C20 N6 174.5(3) . . . . ?
Zn1 O2 C20 C19 -6.3(6) . . . . ?
C21 N6 C20 O2 179.8(3) . . . . ?
C21 N6 C20 C19 0.6(5) . . . . ?
C27 C19 C20 O2 -179.2(4) . . . . ?
C18 C19 C20 O2 3.1(6) . . . . ?
C27 C19 C20 N6 0.0(6) . . . . ?
C18 C19 C20 N6 -177.7(3) . . . . ?
C20 N6 C21 C26 -1.5(6) . . . . ?
C20 N6 C21 C22 178.8(4) . . . . ?
N6 C21 C22 C23 178.6(4) . . . . ?
C26 C21 C22 C23 -1.2(7) . . . . ?
C21 C22 C23 C24 2.9(9) . . . . ?
C22 C23 C24 C25 -2.8(10) . . . . ?
C23 C24 C25 C26 1.0(10) . . . . ?
N6 C21 C26 C25 179.7(4) . . . . ?
C22 C21 C26 C25 -0.5(7) . . . . ?
N6 C21 C26 C27 1.7(6) . . . . ?
C22 C21 C26 C27 -178.5(4) . . . . ?
C24 C25 C26 C21 0.6(8) . . . . ?
C24 C25 C26 C27 178.5(5) . . . . ?
C20 C19 C27 C26 0.4(7) . . . . ?
C18 C19 C27 C26 178.2(4) . . . . ?
C21 C26 C27 C19 -1.3(7) . . . . ?
C25 C26 C27 C19 -179.2(5) . . . . ?
C29 N8 C28 N10 1.5(7) . . . . ?
Zn1 N8 C28 N10 -179.7(4) . . . . ?
C29 N8 C28 N7 -178.7(4) . . . . ?
Zn1 N8 C28 N7 0.2(5) . . . . ?
N4 N7 C28 N8 -5.3(6) . . . . ?
N4 N7 C28 N10 174.6(4) . . . . ?
C28 N8 C29 C30 -1.5(6) . . . . ?
Zn1 N8 C29 C30 179.9(3) . . . . ?
C28 N8 C29 C34 177.2(4) . . . . ?
Zn1 N8 C29 C34 -1.5(6) . . . . ?
N8 C29 C30 C31 1.4(7) . . . . ?
C34 C29 C30 C31 -177.1(5) . . . . ?
C29 C30 C31 N10 -1.3(8) . . . . ?
C29 C30 C31 C33 -179.7(5) . . . . ?
N8 C28 N10 C31 -1.3(7) . . . . ?
N7 C28 N10 C31 178.9(4) . . . . ?
C30 C31 N10 C28 1.1(8) . . . . ?
C33 C31 N10 C28 179.6(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
C34 H28 O2S 0.96 2.76 3.544(7) 139.9 2_545
C2 H1 N4 0.96 2.86 3.442(7) 120.0 .
C34 H26 N3 0.96 2.81 3.419(6) 121.8 .
C34 H26 N3 0.96 2.81 3.419(6) 121.8 .
C2 H1 N4 0.96 2.86 3.442(7) 120.0 .
C34 H26 N3 0.96 2.81 3.419(6) 121.8 .
C34 H28 O2S 0.96 2.76 3.544(7) 139.9 2_545

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.18
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         1.044
_refine_diff_density_min         -0.849
_refine_diff_density_rms         0.090
####################################################################### 
# 
# 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_r20_42_0m
_database_code_depnum_ccdc_archive 'CCDC 2423118'
loop_
_audit_author_name
_audit_author_address
'Malay Dolai'
;Prabhat Kumar College, West Bengal, India
India
;
_audit_update_record             
;
2025-02-11 deposited with the CCDC.	2025-07-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '4(C16 H15 N5 O), C2 H6 O, 2(C H4 O)'
_chemical_formula_sum            'C68 H74 N20 O7'
_chemical_formula_weight         1283.47

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables 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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'

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

_cell_length_a                   22.6848(12)
_cell_length_b                   18.0621(9)
_cell_length_c                   16.8994(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 115.938(2)
_cell_angle_gamma                90.00
_cell_volume                     6226.8(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    300
_cell_measurement_theta_min      3.27
_cell_measurement_theta_max      57.12

_exptl_crystal_description       rodlike
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2712.0
_exptl_absorpt_coefficient_mu    0.755
_exptl_absorpt_correction_type   Empirical
_exptl_absorpt_correction_T_min  0.881
_exptl_absorpt_correction_T_max  0.963
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_reflns_number            52363
_diffrn_reflns_av_R_equivalents  0.1209
_diffrn_reflns_av_sigmaI/netI    0.0551
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.27
_diffrn_reflns_theta_max         57.12
_reflns_number_total             4223
_reflns_number_gt                3967
_reflns_threshold_expression     >2sigma(I)

_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  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4209
_refine_ls_number_parameters     455
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0676
_refine_ls_wR_factor_ref         0.2210
_refine_ls_wR_factor_gt          0.2187
_refine_ls_goodness_of_fit_ref   1.809
_refine_ls_restrained_S_all      1.809
_refine_ls_shift/su_max          4.983
_refine_ls_shift/su_mean         0.011

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.68961(8) 0.55918(9) 0.49791(11) 0.0261(5) Uani 1 1 d . . .
O2 O 0.81109(9) 0.44286(9) 0.49027(12) 0.0279(5) Uani 1 1 d . . .
O3 O 0.38746(10) 0.44209(13) 0.33993(12) 0.0330(6) Uani 1 1 d . . .
N1 N 0.49072(10) 0.57884(12) 0.41319(13) 0.0241(6) Uani 1 1 d . . .
N2 N 0.46581(10) 0.64823(12) 0.41363(14) 0.0242(6) Uani 1 1 d . . .
N3 N 0.36089(10) 0.59777(12) 0.35333(13) 0.0259(6) Uani 1 1 d . . .
N4 N 0.68116(11) 0.43549(12) 0.47249(14) 0.0238(6) Uani 1 1 d . . .
N5 N 0.37975(10) 0.72915(12) 0.37025(13) 0.0248(6) Uani 1 1 d . . .
N6 N 1.05414(10) 0.40072(11) 0.36153(13) 0.0241(6) Uani 1 1 d . . .
N7 N 0.98024(10) 0.35271(12) 0.41021(13) 0.0229(5) Uani 1 1 d . . .
N8 N 0.95687(10) 0.42273(12) 0.41050(13) 0.0238(6) Uani 1 1 d . . .
N9 N 0.80042(11) 0.56617(11) 0.46068(14) 0.0225(6) Uani 1 1 d . . .
N10 N 1.03821(10) 0.26962(11) 0.37046(13) 0.0218(5) Uani 1 1 d . . .
C1 C 0.64210(15) 0.23959(16) 0.4163(2) 0.0356(7) Uani 1 1 d . . .
H1 H 0.6634 0.1948 0.4145 0.043 Uiso 1 1 calc R . .
C2 C 0.57482(15) 0.23915(16) 0.3921(2) 0.0377(8) Uani 1 1 d . . .
H2 H 0.5507 0.1943 0.3741 0.045 Uiso 1 1 calc R . .
C3 C 0.54368(15) 0.30362(15) 0.39434(19) 0.0340(7) Uani 1 1 d . . .
H3 H 0.4979 0.3032 0.3775 0.041 Uiso 1 1 calc R . .
C4 C 0.57867(13) 0.37025(14) 0.42115(16) 0.0263(6) Uani 1 1 d . . .
C5 C 0.54891(13) 0.43855(14) 0.42432(16) 0.0264(7) Uani 1 1 d . . .
H4 H 0.5032 0.4396 0.4082 0.032 Uiso 1 1 calc R . .
C6 C 0.58410(12) 0.50336(14) 0.44994(16) 0.0242(6) Uani 1 1 d . . .
C7 C 0.55342(13) 0.57382(15) 0.45121(16) 0.0241(6) Uani 1 1 d . . .
H5 H 0.5795 0.6156 0.4799 0.029 Uiso 1 1 calc R . .
C8 C 0.39935(12) 0.65805(14) 0.37713(16) 0.0234(6) Uani 1 1 d . . .
C9 C 0.29604(12) 0.61061(15) 0.31807(16) 0.0280(7) Uani 1 1 d . . .
C10 C 0.25234(14) 0.54355(17) 0.28933(19) 0.0388(8) Uani 1 1 d . . .
H11 H 0.2526 0.5230 0.2358 0.058 Uiso 1 1 calc R . .
H12 H 0.2075 0.5578 0.2774 0.058 Uiso 1 1 calc R . .
H10 H 0.2684 0.5062 0.3361 0.058 Uiso 1 1 calc R . .
C11 C 0.29056(13) 0.81904(16) 0.32488(18) 0.0304(7) Uani 1 1 d . . .
H15 H 0.2984 0.8389 0.3826 0.046 Uiso 1 1 calc R . .
H13 H 0.2435 0.8203 0.2857 0.046 Uiso 1 1 calc R . .
H14 H 0.3142 0.8491 0.2997 0.046 Uiso 1 1 calc R . .
C12 C 0.31453(13) 0.74065(15) 0.33510(16) 0.0257(7) Uani 1 1 d . . .
C13 C 0.27076(13) 0.68097(16) 0.30840(17) 0.0288(7) Uani 1 1 d . . .
H9 H 0.2248 0.6889 0.2842 0.035 Uiso 1 1 calc R . .
C14 C 0.67806(14) 0.30395(14) 0.44271(18) 0.0284(7) Uani 1 1 d . . .
H7 H 0.7237 0.3037 0.4585 0.034 Uiso 1 1 calc R . .
C15 C 0.64671(13) 0.36934(15) 0.44604(16) 0.0256(6) Uani 1 1 d . . .
C16 C 0.65436(13) 0.50244(14) 0.47555(16) 0.0237(6) Uani 1 1 d . . .
C17 C 1.11598(13) 0.31454(15) 0.32339(16) 0.0264(7) Uani 1 1 d . . .
H20 H 1.1488 0.3050 0.3042 0.032 Uiso 1 1 calc R . .
C18 C 1.10000(12) 0.38580(15) 0.33409(16) 0.0247(7) Uani 1 1 d . . .
C19 C 1.02589(11) 0.34145(14) 0.37895(16) 0.0217(6) Uani 1 1 d . . .
C20 C 0.91576(12) 0.42855(14) 0.44350(17) 0.0228(6) Uani 1 1 d . . .
H25 H 0.9057 0.3866 0.4693 0.027 Uiso 1 1 calc R . .
C21 C 0.88450(12) 0.49952(14) 0.44147(16) 0.0228(6) Uani 1 1 d . . .
C22 C 0.90274(12) 0.56341(14) 0.41625(16) 0.0233(6) Uani 1 1 d . . .
H27 H 0.9377 0.5623 0.3996 0.028 Uiso 1 1 calc R . .
C23 C 0.87108(12) 0.63239(14) 0.41395(16) 0.0241(6) Uani 1 1 d . . .
C24 C 0.89063(13) 0.70026(14) 0.39090(16) 0.0262(7) Uani 1 1 d . . .
H31 H 0.9256 0.7009 0.3744 0.031 Uiso 1 1 calc R . .
C25 C 0.85963(13) 0.76488(15) 0.39219(17) 0.0269(7) Uani 1 1 d . . .
H30 H 0.8736 0.8103 0.3776 0.032 Uiso 1 1 calc R . .
C26 C 0.80725(13) 0.76418(15) 0.41511(17) 0.0273(7) Uani 1 1 d . . .
H29 H 0.7857 0.8092 0.4155 0.033 Uiso 1 1 calc R . .
C27 C 0.81880(12) 0.63220(14) 0.43725(15) 0.0228(6) Uani 1 1 d . . .
C28 C 0.78647(13) 0.69848(14) 0.43713(17) 0.0253(7) Uani 1 1 d . . .
H28 H 0.7507 0.6983 0.4520 0.030 Uiso 1 1 calc R . .
C29 C 0.83062(12) 0.50011(14) 0.46583(16) 0.0223(6) Uani 1 1 d . . .
C30 C 1.13192(14) 0.45049(16) 0.31301(19) 0.0330(7) Uani 1 1 d . . .
H33 H 1.1053 0.4660 0.2520 0.049 Uiso 1 1 calc R . .
H32 H 1.1757 0.4362 0.3204 0.049 Uiso 1 1 calc R . .
H34 H 1.1357 0.4916 0.3528 0.049 Uiso 1 1 calc R . .
C31 C 1.08348(12) 0.25653(15) 0.34107(16) 0.0237(6) Uani 1 1 d . . .
C32 C 1.09829(13) 0.17756(15) 0.32922(17) 0.0280(7) Uani 1 1 d . . .
H22 H 1.1263 0.1559 0.3867 0.042 Uiso 1 1 calc R . .
H21 H 1.1210 0.1756 0.2915 0.042 Uiso 1 1 calc R . .
H23 H 1.0573 0.1495 0.3017 0.042 Uiso 1 1 calc R . .
C33 C 0.38263(19) 0.44013(19) 0.2542(2) 0.0509(9) Uani 1 1 d . . .
H19 H 0.3401 0.4601 0.2129 0.076 Uiso 1 1 calc R . .
H18 H 0.3867 0.3889 0.2382 0.076 Uiso 1 1 calc R . .
H17 H 0.4178 0.4701 0.2517 0.076 Uiso 1 1 calc R . .
H24 H 0.9542(14) 0.3154(16) 0.4122(18) 0.030(8) Uiso 1 1 d . . .
H8 H 0.4902(14) 0.6876(16) 0.4169(18) 0.027(8) Uiso 1 1 d . . .
H16 H 0.3864(15) 0.4824(18) 0.351(2) 0.036(10) Uiso 1 1 d . . .
O4 O 0.0000 0.5741(4) 0.2500 0.163(3) Uani 1 2 d S . .
H39 H 0.769(2) 0.5688(19) 0.473(3) 0.065(12) Uiso 1 1 d . . .
H40 H 0.7230(16) 0.4343(14) 0.4813(17) 0.023(7) Uiso 1 1 d . . .
C40 C 0.01874(17) 0.55881(16) 0.3435(2) 0.0400(8) Uani 1 1 d . . .
H40A H 0.0046 0.5999 0.3690 0.060 Uiso 1 1 calc R . .
H40B H 0.0665 0.5534 0.3750 0.060 Uiso 1 1 calc R . .
H40C H -0.0023 0.5129 0.3488 0.060 Uiso 1 1 calc R . .


_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 C16 1.252(3) . ?
O2 C29 1.263(3) . ?
O3 C33 1.405(4) . ?
O3 H16 0.76(3) . ?
N1 C7 1.282(3) . ?
N1 N2 1.376(3) . ?
N2 C8 1.368(3) . ?
N2 H8 0.89(3) . ?
N3 C8 1.342(3) . ?
N3 C9 1.344(3) . ?
N4 C16 1.365(3) . ?
N4 C15 1.390(3) . ?
N4 H40 0.89(3) . ?
N5 C8 1.347(3) . ?
N5 C12 1.348(3) . ?
N6 C18 1.338(3) . ?
N6 C19 1.345(3) . ?
N7 C19 1.368(3) . ?
N7 N8 1.372(3) . ?
N7 H24 0.91(3) . ?
N8 C20 1.283(3) . ?
N9 C29 1.360(3) . ?
N9 C27 1.378(3) . ?
N9 H39 0.83(4) . ?
N10 C31 1.343(3) . ?
N10 C19 1.348(3) . ?
C1 C14 1.377(4) . ?
C1 C2 1.397(4) . ?
C1 H1 0.9500 . ?
C2 C3 1.371(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.403(4) . ?
C3 H3 0.9500 . ?
C4 C15 1.411(4) . ?
C4 C5 1.418(4) . ?
C5 C6 1.376(4) . ?
C5 H4 0.9500 . ?
C6 C7 1.455(4) . ?
C6 C16 1.457(4) . ?
C7 H5 0.9500 . ?
C9 C13 1.374(4) . ?
C9 C10 1.505(4) . ?
C10 H11 0.9800 . ?
C10 H12 0.9800 . ?
C10 H10 0.9800 . ?
C11 C12 1.499(4) . ?
C11 H15 0.9800 . ?
C11 H13 0.9800 . ?
C11 H14 0.9800 . ?
C12 C13 1.400(4) . ?
C13 H9 0.9500 . ?
C14 C15 1.392(4) . ?
C14 H7 0.9500 . ?
C17 C18 1.371(4) . ?
C17 C31 1.387(4) . ?
C17 H20 0.9500 . ?
C18 C30 1.497(4) . ?
C20 C21 1.458(3) . ?
C20 H25 0.9500 . ?
C21 C22 1.356(3) . ?
C21 C29 1.451(4) . ?
C22 C23 1.430(4) . ?
C22 H27 0.9500 . ?
C23 C27 1.404(4) . ?
C23 C24 1.415(4) . ?
C24 C25 1.368(4) . ?
C24 H31 0.9500 . ?
C25 C26 1.402(4) . ?
C25 H30 0.9500 . ?
C26 C28 1.386(4) . ?
C26 H29 0.9500 . ?
C27 C28 1.403(4) . ?
C28 H28 0.9500 . ?
C30 H33 0.9800 . ?
C30 H32 0.9800 . ?
C30 H34 0.9800 . ?
C31 C32 1.499(4) . ?
C32 H22 0.9800 . ?
C32 H21 0.9800 . ?
C32 H23 0.9800 . ?
C33 H19 0.9800 . ?
C33 H18 0.9800 . ?
C33 H17 0.9800 . ?
O4 C40 1.471(3) 2 ?
O4 C40 1.471(3) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 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
C33 O3 H16 107(3) . . ?
C7 N1 N2 115.5(2) . . ?
C8 N2 N1 119.3(2) . . ?
C8 N2 H8 117.3(18) . . ?
N1 N2 H8 118.9(18) . . ?
C8 N3 C9 115.8(2) . . ?
C16 N4 C15 125.2(2) . . ?
C16 N4 H40 118.2(17) . . ?
C15 N4 H40 116.1(17) . . ?
C8 N5 C12 116.2(2) . . ?
C18 N6 C19 115.6(2) . . ?
C19 N7 N8 119.8(2) . . ?
C19 N7 H24 121.3(18) . . ?
N8 N7 H24 115.3(18) . . ?
C20 N8 N7 115.6(2) . . ?
C29 N9 C27 124.8(2) . . ?
C29 N9 H39 120(3) . . ?
C27 N9 H39 115(3) . . ?
C31 N10 C19 115.9(2) . . ?
C14 C1 C2 121.1(3) . . ?
C14 C1 H1 119.5 . . ?
C2 C1 H1 119.5 . . ?
C3 C2 C1 119.8(3) . . ?
C3 C2 H2 120.1 . . ?
C1 C2 H2 120.1 . . ?
C2 C3 C4 120.8(3) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 H3 119.6 . . ?
C3 C4 C15 118.5(2) . . ?
C3 C4 C5 123.1(2) . . ?
C15 C4 C5 118.4(2) . . ?
C6 C5 C4 122.1(2) . . ?
C6 C5 H4 118.9 . . ?
C4 C5 H4 118.9 . . ?
C5 C6 C7 122.2(2) . . ?
C5 C6 C16 119.5(2) . . ?
C7 C6 C16 118.3(2) . . ?
N1 C7 C6 119.2(2) . . ?
N1 C7 H5 120.4 . . ?
C6 C7 H5 120.4 . . ?
N3 C8 N5 126.9(2) . . ?
N3 C8 N2 118.3(2) . . ?
N5 C8 N2 114.8(2) . . ?
N3 C9 C13 122.1(2) . . ?
N3 C9 C10 116.3(2) . . ?
C13 C9 C10 121.6(2) . . ?
C9 C10 H11 109.5 . . ?
C9 C10 H12 109.5 . . ?
H11 C10 H12 109.5 . . ?
C9 C10 H10 109.5 . . ?
H11 C10 H10 109.5 . . ?
H12 C10 H10 109.5 . . ?
C12 C11 H15 109.5 . . ?
C12 C11 H13 109.5 . . ?
H15 C11 H13 109.5 . . ?
C12 C11 H14 109.5 . . ?
H15 C11 H14 109.5 . . ?
H13 C11 H14 109.5 . . ?
N5 C12 C13 120.7(2) . . ?
N5 C12 C11 118.0(2) . . ?
C13 C12 C11 121.3(2) . . ?
C9 C13 C12 118.3(2) . . ?
C9 C13 H9 120.9 . . ?
C12 C13 H9 120.9 . . ?
C1 C14 C15 119.2(3) . . ?
C1 C14 H7 120.4 . . ?
C15 C14 H7 120.4 . . ?
N4 C15 C14 121.1(2) . . ?
N4 C15 C4 118.3(2) . . ?
C14 C15 C4 120.6(2) . . ?
O1 C16 N4 120.0(2) . . ?
O1 C16 C6 123.5(2) . . ?
N4 C16 C6 116.5(2) . . ?
C18 C17 C31 119.0(2) . . ?
C18 C17 H20 120.5 . . ?
C31 C17 H20 120.5 . . ?
N6 C18 C17 121.7(2) . . ?
N6 C18 C30 117.1(2) . . ?
C17 C18 C30 121.2(2) . . ?
N6 C19 N10 127.0(2) . . ?
N6 C19 N7 118.7(2) . . ?
N10 C19 N7 114.3(2) . . ?
N8 C20 C21 120.0(2) . . ?
N8 C20 H25 120.0 . . ?
C21 C20 H25 120.0 . . ?
C22 C21 C29 119.6(2) . . ?
C22 C21 C20 122.9(2) . . ?
C29 C21 C20 117.5(2) . . ?
C21 C22 C23 122.1(2) . . ?
C21 C22 H27 118.9 . . ?
C23 C22 H27 118.9 . . ?
C27 C23 C24 119.0(2) . . ?
C27 C23 C22 117.8(2) . . ?
C24 C23 C22 123.2(2) . . ?
C25 C24 C23 120.6(2) . . ?
C25 C24 H31 119.7 . . ?
C23 C24 H31 119.7 . . ?
C24 C25 C26 120.0(2) . . ?
C24 C25 H30 120.0 . . ?
C26 C25 H30 120.0 . . ?
C28 C26 C25 120.7(2) . . ?
C28 C26 H29 119.6 . . ?
C25 C26 H29 119.6 . . ?
N9 C27 C23 118.8(2) . . ?
N9 C27 C28 121.0(2) . . ?
C23 C27 C28 120.2(2) . . ?
C26 C28 C27 119.4(2) . . ?
C26 C28 H28 120.3 . . ?
C27 C28 H28 120.3 . . ?
O2 C29 N9 120.0(2) . . ?
O2 C29 C21 123.1(2) . . ?
N9 C29 C21 116.9(2) . . ?
C18 C30 H33 109.5 . . ?
C18 C30 H32 109.5 . . ?
H33 C30 H32 109.5 . . ?
C18 C30 H34 109.5 . . ?
H33 C30 H34 109.5 . . ?
H32 C30 H34 109.5 . . ?
N10 C31 C17 120.7(2) . . ?
N10 C31 C32 118.0(2) . . ?
C17 C31 C32 121.3(2) . . ?
C31 C32 H22 109.5 . . ?
C31 C32 H21 109.5 . . ?
H22 C32 H21 109.5 . . ?
C31 C32 H23 109.5 . . ?
H22 C32 H23 109.5 . . ?
H21 C32 H23 109.5 . . ?
O3 C33 H19 109.5 . . ?
O3 C33 H18 109.5 . . ?
H19 C33 H18 109.5 . . ?
O3 C33 H17 109.5 . . ?
H19 C33 H17 109.5 . . ?
H18 C33 H17 109.5 . . ?
C40 O4 C40 158.4(6) 2 . ?
O4 C40 H40A 109.5 . . ?
O4 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
O4 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 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
C7 N1 N2 C8 -177.8(2) . . . . ?
C19 N7 N8 C20 -177.9(2) . . . . ?
C14 C1 C2 C3 0.1(5) . . . . ?
C1 C2 C3 C4 -0.3(4) . . . . ?
C2 C3 C4 C15 -0.2(4) . . . . ?
C2 C3 C4 C5 179.7(3) . . . . ?
C3 C4 C5 C6 -179.3(2) . . . . ?
C15 C4 C5 C6 0.6(4) . . . . ?
C4 C5 C6 C7 178.5(2) . . . . ?
C4 C5 C6 C16 -0.6(4) . . . . ?
N2 N1 C7 C6 -176.9(2) . . . . ?
C5 C6 C7 N1 -12.5(4) . . . . ?
C16 C6 C7 N1 166.5(2) . . . . ?
C9 N3 C8 N5 0.8(4) . . . . ?
C9 N3 C8 N2 179.8(2) . . . . ?
C12 N5 C8 N3 -0.5(4) . . . . ?
C12 N5 C8 N2 -179.5(2) . . . . ?
N1 N2 C8 N3 9.3(3) . . . . ?
N1 N2 C8 N5 -171.6(2) . . . . ?
C8 N3 C9 C13 -1.1(4) . . . . ?
C8 N3 C9 C10 178.7(2) . . . . ?
C8 N5 C12 C13 0.4(3) . . . . ?
C8 N5 C12 C11 -179.0(2) . . . . ?
N3 C9 C13 C12 1.1(4) . . . . ?
C10 C9 C13 C12 -178.7(2) . . . . ?
N5 C12 C13 C9 -0.7(4) . . . . ?
C11 C12 C13 C9 178.7(2) . . . . ?
C2 C1 C14 C15 0.6(4) . . . . ?
C16 N4 C15 C14 178.2(2) . . . . ?
C16 N4 C15 C4 -0.8(4) . . . . ?
C1 C14 C15 N4 179.9(2) . . . . ?
C1 C14 C15 C4 -1.2(4) . . . . ?
C3 C4 C15 N4 179.9(2) . . . . ?
C5 C4 C15 N4 0.0(3) . . . . ?
C3 C4 C15 C14 1.0(4) . . . . ?
C5 C4 C15 C14 -178.9(2) . . . . ?
C15 N4 C16 O1 -177.8(2) . . . . ?
C15 N4 C16 C6 0.9(4) . . . . ?
C5 C6 C16 O1 178.5(2) . . . . ?
C7 C6 C16 O1 -0.6(4) . . . . ?
C5 C6 C16 N4 -0.2(3) . . . . ?
C7 C6 C16 N4 -179.2(2) . . . . ?
C19 N6 C18 C17 1.0(3) . . . . ?
C19 N6 C18 C30 179.3(2) . . . . ?
C31 C17 C18 N6 0.3(4) . . . . ?
C31 C17 C18 C30 -177.9(2) . . . . ?
C18 N6 C19 N10 -1.0(4) . . . . ?
C18 N6 C19 N7 177.7(2) . . . . ?
C31 N10 C19 N6 -0.3(3) . . . . ?
C31 N10 C19 N7 -179.1(2) . . . . ?
N8 N7 C19 N6 9.9(3) . . . . ?
N8 N7 C19 N10 -171.1(2) . . . . ?
N7 N8 C20 C21 -175.8(2) . . . . ?
N8 C20 C21 C22 -8.8(4) . . . . ?
N8 C20 C21 C29 169.8(2) . . . . ?
C29 C21 C22 C23 0.9(4) . . . . ?
C20 C21 C22 C23 179.4(2) . . . . ?
C21 C22 C23 C27 -1.2(4) . . . . ?
C21 C22 C23 C24 177.7(2) . . . . ?
C27 C23 C24 C25 0.7(4) . . . . ?
C22 C23 C24 C25 -178.2(2) . . . . ?
C23 C24 C25 C26 -1.1(4) . . . . ?
C24 C25 C26 C28 0.4(4) . . . . ?
C29 N9 C27 C23 2.2(4) . . . . ?
C29 N9 C27 C28 -177.3(2) . . . . ?
C24 C23 C27 N9 -179.2(2) . . . . ?
C22 C23 C27 N9 -0.3(3) . . . . ?
C24 C23 C27 C28 0.3(3) . . . . ?
C22 C23 C27 C28 179.3(2) . . . . ?
C25 C26 C28 C27 0.6(4) . . . . ?
N9 C27 C28 C26 178.5(2) . . . . ?
C23 C27 C28 C26 -1.0(4) . . . . ?
C27 N9 C29 O2 178.1(2) . . . . ?
C27 N9 C29 C21 -2.4(3) . . . . ?
C22 C21 C29 O2 -179.7(2) . . . . ?
C20 C21 C29 O2 1.7(3) . . . . ?
C22 C21 C29 N9 0.8(3) . . . . ?
C20 C21 C29 N9 -177.8(2) . . . . ?
C19 N10 C31 C17 1.7(3) . . . . ?
C19 N10 C31 C32 -179.1(2) . . . . ?
C18 C17 C31 N10 -1.7(4) . . . . ?
C18 C17 C31 C32 179.1(2) . . . . ?

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
C32 H22 O1 0.98 2.51 3.439(3) 158.7 3_545
C30 H33 N8 0.98 2.60 3.453(4) 145.6 2_755
C11 H15 O2 0.98 2.54 3.448(3) 153.9 3_455

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        57.12
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.310
_refine_diff_density_min         -0.890
_refine_diff_density_rms         0.102
