# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry.
# 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_JR749
_database_code_depnum_ccdc_archive 'CCDC 1884529'
loop_
_audit_author_name
_audit_author_address
'Dr. P. K. SUTHADEVI ANTHARJANAM'
;IIT madras
India
;
_audit_update_record             
;
2018-12-12 deposited with the CCDC.	2020-05-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H19 N O6'
_chemical_formula_sum            'C24 H19 N O6'
_chemical_formula_weight         417.40

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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   8.2622(7)
_cell_length_b                   10.8562(10)
_cell_length_c                   11.4554(8)
_cell_angle_alpha                83.258(4)
_cell_angle_beta                 82.820(4)
_cell_angle_gamma                84.193(4)
_cell_volume                     1008.49(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4080
_cell_measurement_theta_min      2.49
_cell_measurement_theta_max      24.38

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_F_000             436
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    0.100
_shelx_estimated_absorpt_T_min   0.980
_shelx_estimated_absorpt_T_max   0.985
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6961
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_process_details   'SADABS (Bruker, 2004)'
_exptl_absorpt_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 axs kappa apex2 CCD Diffractometer'
_diffrn_measurement_method       'ω and φ scan'


_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15132
_diffrn_reflns_av_unetI/netI     0.0371
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.474
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_full        24.997
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3551
_reflns_number_gt                2255
_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       'APEX2 (Bruker, 2004)'
_computing_cell_refinement       'APEX2/SAINT (Bruker, 2004)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2004)'
_computing_structure_solution    'SHELXT-2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    
'ORTEP3 (Farrugia, 1997) and Mercury (Bruno et al., 2002)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'


_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)+(0.0550P)²+0.2718P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.008(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3551
_refine_ls_number_parameters     284
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0828
_refine_ls_R_factor_gt           0.0433
_refine_ls_wR_factor_ref         0.1287
_refine_ls_wR_factor_gt          0.1025
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.051
_refine_ls_shift/su_max          0.000
_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
C1 C 0.1298(3) 0.6108(2) 0.56929(19) 0.0399(5) Uani 1 1 d . . . . .
C2 C 0.0383(3) 0.7017(2) 0.6278(2) 0.0516(7) Uani 1 1 d . . . . .
H2 H 0.0252 0.6985 0.7099 0.062 Uiso 1 1 calc R U . . .
C3 C -0.0329(3) 0.7983(2) 0.5573(3) 0.0597(7) Uani 1 1 d . . . . .
H3 H -0.0950 0.8630 0.5929 0.072 Uiso 1 1 calc R U . . .
C4 C -0.0152(3) 0.8022(2) 0.4357(2) 0.0580(7) Uani 1 1 d . . . . .
H4 H -0.0661 0.8690 0.3914 0.070 Uiso 1 1 calc R U . . .
C5 C 0.0763(3) 0.7092(2) 0.3783(2) 0.0524(6) Uani 1 1 d . . . . .
H5 H 0.0875 0.7114 0.2963 0.063 Uiso 1 1 calc R U . . .
C6 C 0.1506(3) 0.6128(2) 0.44780(19) 0.0393(5) Uani 1 1 d . . . . .
C7 C 0.2877(3) 0.44977(19) 0.51885(18) 0.0363(5) Uani 1 1 d . U . . .
C8 C 0.3994(2) 0.33588(18) 0.52906(17) 0.0330(5) Uani 1 1 d . . . . .
C9 C 0.4676(3) 0.29340(19) 0.42210(18) 0.0358(5) Uani 1 1 d . . . . .
H9 H 0.4400 0.3375 0.3517 0.043 Uiso 1 1 calc R U . . .
C10 C 0.5746(3) 0.18809(19) 0.41787(17) 0.0364(5) Uani 1 1 d . . . . .
C11 C 0.6168(3) 0.12336(19) 0.52257(18) 0.0388(5) Uani 1 1 d . . . . .
H11 H 0.6882 0.0515 0.5207 0.047 Uiso 1 1 calc R U . . .
C12 C 0.5535(3) 0.16486(19) 0.63014(17) 0.0365(5) Uani 1 1 d . . . . .
C13 C 0.4412(3) 0.27085(19) 0.63651(17) 0.0330(5) Uani 1 1 d . . . . .
C14 C 0.3640(3) 0.30550(19) 0.75395(17) 0.0351(5) Uani 1 1 d . . . . .
C15 C 0.2453(3) 0.2347(2) 0.81668(18) 0.0408(6) Uani 1 1 d . . . . .
H15 H 0.2167 0.1656 0.7856 0.049 Uiso 1 1 calc R U . . .
C16 C 0.1692(3) 0.2655(2) 0.92458(18) 0.0458(6) Uani 1 1 d . . . . .
H16 H 0.0893 0.2173 0.9656 0.055 Uiso 1 1 calc R U . . .
C17 C 0.2107(3) 0.3671(2) 0.97223(18) 0.0422(6) Uani 1 1 d . . . . .
C18 C 0.3310(3) 0.4367(2) 0.91217(19) 0.0470(6) Uani 1 1 d . . . . .
H18 H 0.3618 0.5043 0.9444 0.056 Uiso 1 1 calc R U . . .
C19 C 0.4061(3) 0.4054(2) 0.80321(19) 0.0437(6) Uani 1 1 d . . . . .
H19 H 0.4867 0.4532 0.7626 0.052 Uiso 1 1 calc R U . . .
C20 C 0.1649(4) 0.4940(3) 1.1316(2) 0.0784(9) Uani 1 1 d . . . . .
H20A H 0.2755 0.4801 1.1510 0.118 Uiso 1 1 calc R U . . .
H20B H 0.0915 0.5042 1.2024 0.118 Uiso 1 1 calc R U . . .
H20C H 0.1542 0.5679 1.0772 0.118 Uiso 1 1 calc R U . . .
C21 C 0.6186(3) 0.1005(2) 0.7398(2) 0.0487(6) Uani 1 1 d . . . . .
C22 C 0.7398(5) -0.0866(3) 0.8275(3) 0.1042(13) Uani 1 1 d . . . . .
H22A H 0.8436 -0.0551 0.8302 0.156 Uiso 1 1 calc R U . . .
H22B H 0.7563 -0.1735 0.8169 0.156 Uiso 1 1 calc R U . . .
H22C H 0.6713 -0.0756 0.9003 0.156 Uiso 1 1 calc R U . . .
C23 C 0.6521(3) 0.1437(2) 0.30443(19) 0.0457(6) Uani 1 1 d . . . . .
C24 C 0.6766(5) 0.1821(3) 0.0960(2) 0.0984(12) Uani 1 1 d . . . . .
H24A H 0.7919 0.1917 0.0850 0.148 Uiso 1 1 calc R U . . .
H24B H 0.6245 0.2342 0.0353 0.148 Uiso 1 1 calc R U . . .
H24C H 0.6593 0.0968 0.0915 0.148 Uiso 1 1 calc R U . . .
N1 N 0.2532(2) 0.50845(15) 0.41852(14) 0.0372(4) Uani 1 1 d . U . . .
O1 O 0.1260(2) 0.39088(16) 1.07901(13) 0.0607(5) Uani 1 1 d . . . . .
O2 O 0.21743(19) 0.50499(14) 0.61529(12) 0.0468(4) Uani 1 1 d . . . . .
O3 O 0.6393(3) 0.14926(18) 0.82354(16) 0.0833(7) Uani 1 1 d . . . . .
O4 O 0.6614(3) -0.01927(17) 0.72953(15) 0.0738(6) Uani 1 1 d . . . . .
O5 O 0.7452(2) 0.05178(16) 0.29686(14) 0.0643(5) Uani 1 1 d . . . . .
O6 O 0.6074(2) 0.21795(15) 0.21076(13) 0.0652(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
C1 C2 1.368(3) . ?
C1 C6 1.379(3) . ?
C1 O2 1.381(2) . ?
C2 C3 1.375(3) . ?
C2 H2 0.9300 . ?
C3 C4 1.379(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.378(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.380(3) . ?
C5 H5 0.9300 . ?
C6 N1 1.392(3) . ?
C7 N1 1.297(3) . ?
C7 O2 1.357(2) . ?
C7 C8 1.468(3) . ?
C8 C9 1.392(3) . ?
C8 C13 1.409(3) . ?
C9 C10 1.374(3) . ?
C9 H9 0.9300 . ?
C10 C11 1.383(3) . ?
C10 C23 1.486(3) . ?
C11 C12 1.384(3) . ?
C11 H11 0.9300 . ?
C12 C13 1.406(3) . ?
C12 C21 1.497(3) . ?
C13 C14 1.488(3) . ?
C14 C19 1.373(3) . ?
C14 C15 1.384(3) . ?
C15 C16 1.377(3) . ?
C15 H15 0.9300 . ?
C16 C17 1.378(3) . ?
C16 H16 0.9300 . ?
C17 O1 1.369(2) . ?
C17 C18 1.375(3) . ?
C18 C19 1.386(3) . ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?
C20 O1 1.414(3) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 O3 1.187(3) . ?
C21 O4 1.327(3) . ?
C22 O4 1.451(3) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 O5 1.201(3) . ?
C23 O6 1.332(3) . ?
C24 O6 1.447(3) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 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
C2 C1 C6 123.4(2) . . ?
C2 C1 O2 128.9(2) . . ?
C6 C1 O2 107.66(18) . . ?
C1 C2 C3 115.7(2) . . ?
C1 C2 H2 122.2 . . ?
C3 C2 H2 122.2 . . ?
C2 C3 C4 122.1(2) . . ?
C2 C3 H3 118.9 . . ?
C4 C3 H3 118.9 . . ?
C5 C4 C3 121.4(2) . . ?
C5 C4 H4 119.3 . . ?
C3 C4 H4 119.3 . . ?
C4 C5 C6 117.1(2) . . ?
C4 C5 H5 121.5 . . ?
C6 C5 H5 121.5 . . ?
C1 C6 C5 120.2(2) . . ?
C1 C6 N1 108.23(18) . . ?
C5 C6 N1 131.5(2) . . ?
N1 C7 O2 114.54(18) . . ?
N1 C7 C8 123.52(18) . . ?
O2 C7 C8 121.88(18) . . ?
C9 C8 C13 119.82(18) . . ?
C9 C8 C7 115.23(18) . . ?
C13 C8 C7 124.95(18) . . ?
C10 C9 C8 121.74(19) . . ?
C10 C9 H9 119.1 . . ?
C8 C9 H9 119.1 . . ?
C9 C10 C11 119.10(19) . . ?
C9 C10 C23 122.36(19) . . ?
C11 C10 C23 118.50(19) . . ?
C10 C11 C12 120.41(19) . . ?
C10 C11 H11 119.8 . . ?
C12 C11 H11 119.8 . . ?
C11 C12 C13 121.37(18) . . ?
C11 C12 C21 118.18(19) . . ?
C13 C12 C21 120.24(18) . . ?
C12 C13 C8 117.53(18) . . ?
C12 C13 C14 119.69(17) . . ?
C8 C13 C14 122.66(18) . . ?
C19 C14 C15 118.3(2) . . ?
C19 C14 C13 122.5(2) . . ?
C15 C14 C13 119.16(19) . . ?
C16 C15 C14 120.7(2) . . ?
C16 C15 H15 119.7 . . ?
C14 C15 H15 119.7 . . ?
C15 C16 C17 120.4(2) . . ?
C15 C16 H16 119.8 . . ?
C17 C16 H16 119.8 . . ?
O1 C17 C18 124.6(2) . . ?
O1 C17 C16 115.9(2) . . ?
C18 C17 C16 119.5(2) . . ?
C17 C18 C19 119.6(2) . . ?
C17 C18 H18 120.2 . . ?
C19 C18 H18 120.2 . . ?
C14 C19 C18 121.4(2) . . ?
C14 C19 H19 119.3 . . ?
C18 C19 H19 119.3 . . ?
O1 C20 H20A 109.5 . . ?
O1 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
O1 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O3 C21 O4 123.0(2) . . ?
O3 C21 C12 125.6(2) . . ?
O4 C21 C12 111.31(19) . . ?
O4 C22 H22A 109.5 . . ?
O4 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
O4 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O5 C23 O6 123.3(2) . . ?
O5 C23 C10 124.4(2) . . ?
O6 C23 C10 112.30(19) . . ?
O6 C24 H24A 109.5 . . ?
O6 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
O6 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C7 N1 C6 105.18(17) . . ?
C17 O1 C20 117.9(2) . . ?
C7 O2 C1 104.39(16) . . ?
C21 O4 C22 115.0(2) . . ?
C23 O6 C24 116.4(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 -0.4(4) . . . . ?
O2 C1 C2 C3 178.6(2) . . . . ?
C1 C2 C3 C4 0.9(4) . . . . ?
C2 C3 C4 C5 -0.4(4) . . . . ?
C3 C4 C5 C6 -0.6(4) . . . . ?
C2 C1 C6 C5 -0.6(4) . . . . ?
O2 C1 C6 C5 -179.8(2) . . . . ?
C2 C1 C6 N1 178.5(2) . . . . ?
O2 C1 C6 N1 -0.7(2) . . . . ?
C4 C5 C6 C1 1.1(3) . . . . ?
C4 C5 C6 N1 -177.9(2) . . . . ?
N1 C7 C8 C9 -0.1(3) . . . . ?
O2 C7 C8 C9 -177.21(19) . . . . ?
N1 C7 C8 C13 179.1(2) . . . . ?
O2 C7 C8 C13 2.0(3) . . . . ?
C13 C8 C9 C10 0.6(3) . . . . ?
C7 C8 C9 C10 179.9(2) . . . . ?
C8 C9 C10 C11 -0.6(3) . . . . ?
C8 C9 C10 C23 -178.2(2) . . . . ?
C9 C10 C11 C12 -0.7(3) . . . . ?
C23 C10 C11 C12 176.9(2) . . . . ?
C10 C11 C12 C13 2.0(3) . . . . ?
C10 C11 C12 C21 -172.7(2) . . . . ?
C11 C12 C13 C8 -2.0(3) . . . . ?
C21 C12 C13 C8 172.6(2) . . . . ?
C11 C12 C13 C14 174.2(2) . . . . ?
C21 C12 C13 C14 -11.1(3) . . . . ?
C9 C8 C13 C12 0.7(3) . . . . ?
C7 C8 C13 C12 -178.5(2) . . . . ?
C9 C8 C13 C14 -175.4(2) . . . . ?
C7 C8 C13 C14 5.4(3) . . . . ?
C12 C13 C14 C19 107.1(2) . . . . ?
C8 C13 C14 C19 -76.9(3) . . . . ?
C12 C13 C14 C15 -72.8(3) . . . . ?
C8 C13 C14 C15 103.2(2) . . . . ?
C19 C14 C15 C16 1.3(3) . . . . ?
C13 C14 C15 C16 -178.78(19) . . . . ?
C14 C15 C16 C17 -0.3(3) . . . . ?
C15 C16 C17 O1 179.03(19) . . . . ?
C15 C16 C17 C18 -1.2(3) . . . . ?
O1 C17 C18 C19 -178.6(2) . . . . ?
C16 C17 C18 C19 1.6(3) . . . . ?
C15 C14 C19 C18 -0.9(3) . . . . ?
C13 C14 C19 C18 179.2(2) . . . . ?
C17 C18 C19 C14 -0.6(3) . . . . ?
C11 C12 C21 O3 143.8(3) . . . . ?
C13 C12 C21 O3 -31.0(4) . . . . ?
C11 C12 C21 O4 -32.1(3) . . . . ?
C13 C12 C21 O4 153.0(2) . . . . ?
C9 C10 C23 O5 -179.5(2) . . . . ?
C11 C10 C23 O5 3.0(4) . . . . ?
C9 C10 C23 O6 0.9(3) . . . . ?
C11 C10 C23 O6 -176.7(2) . . . . ?
O2 C7 N1 C6 0.0(2) . . . . ?
C8 C7 N1 C6 -177.32(19) . . . . ?
C1 C6 N1 C7 0.4(2) . . . . ?
C5 C6 N1 C7 179.5(2) . . . . ?
C18 C17 O1 C20 -0.1(3) . . . . ?
C16 C17 O1 C20 179.7(2) . . . . ?
N1 C7 O2 C1 -0.4(2) . . . . ?
C8 C7 O2 C1 176.97(19) . . . . ?
C2 C1 O2 C7 -178.5(2) . . . . ?
C6 C1 O2 C7 0.6(2) . . . . ?
O3 C21 O4 C22 -1.4(4) . . . . ?
C12 C21 O4 C22 174.6(2) . . . . ?
O5 C23 O6 C24 0.4(4) . . . . ?
C10 C23 O6 C24 -179.9(2) . . . . ?

_refine_diff_density_max         0.242
_refine_diff_density_min         -0.195
_refine_diff_density_rms         0.039

####################################################################### 
# 
# 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_JR637
_database_code_depnum_ccdc_archive 'CCDC 1884531'
loop_
_audit_author_name
_audit_author_address
'Dr. P. K. SUTHADEVI ANTHARJANAM'
;IIT madras
India
;
_audit_update_record             
;
2018-12-12 deposited with the CCDC.	2020-05-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C33 H30 Cl N3 O9'
_chemical_formula_sum            'C33 H30 Cl N3 O9'
_chemical_formula_weight         648.05

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   9.3935(6)
_cell_length_b                   10.3136(7)
_cell_length_c                   17.8351(12)
_cell_angle_alpha                102.592(3)
_cell_angle_beta                 95.138(4)
_cell_angle_gamma                101.978(3)
_cell_volume                     1633.08(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9858
_cell_measurement_theta_min      3.01
_cell_measurement_theta_max      26.07

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_F_000             676
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.175
_shelx_estimated_absorpt_T_min   0.974
_shelx_estimated_absorpt_T_max   0.983
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7151
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   'SADABS (Bruker, 2016)'
_exptl_absorpt_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 axs kappa apex3 CMOS Diffractometer'
_diffrn_measurement_method       'ω and φ scan'

_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            46502
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_av_R_equivalents  0.0555
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.018
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             5738
_reflns_number_gt                4161
_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       'APEX3(Bruker, 2016)'
_computing_cell_refinement       'APEX3/SAINT (Bruker, 2016)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2016)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    
'ORTEP3 (Farrugia, 1997) and Mercury (Bruno et al., 2002)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'


_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)+(0.0729P)²+0.4651P] 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-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.032(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         5738
_refine_ls_number_parameters     420
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0498
_refine_ls_wR_factor_ref         0.1504
_refine_ls_wR_factor_gt          0.1267
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_restrained_S_all      1.080
_refine_ls_shift/su_max          0.000
_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
C1 C 0.2386(5) 0.1573(7) 0.3578(2) 0.174(3) Uani 1 1 d . . . . .
H1A H 0.1813 0.1288 0.3072 0.260 Uiso 1 1 calc R U . . .
H1B H 0.3239 0.2272 0.3578 0.260 Uiso 1 1 calc R U . . .
H1C H 0.2687 0.0806 0.3708 0.260 Uiso 1 1 calc R U . . .
C2 C 0.0129(5) 0.1091(5) 0.4189(2) 0.155(2) Uani 1 1 d . . . . .
H2A H -0.0473 0.0819 0.3691 0.233 Uiso 1 1 calc R U . . .
H2B H 0.0401 0.0309 0.4315 0.233 Uiso 1 1 calc R U . . .
H2C H -0.0411 0.1480 0.4576 0.233 Uiso 1 1 calc R U . . .
C3 C 0.0999(6) 0.3339(5) 0.3973(2) 0.1486(19) Uani 1 1 d . . . . .
H3A H 0.0396 0.3059 0.3476 0.223 Uiso 1 1 calc R U . . .
H3B H 0.0446 0.3700 0.4362 0.223 Uiso 1 1 calc R U . . .
H3C H 0.1849 0.4030 0.3960 0.223 Uiso 1 1 calc R U . . .
C4 C 0.1478(3) 0.2126(3) 0.41644(14) 0.0740(8) Uani 1 1 d . . . . .
C5 C 0.2085(3) 0.3156(2) 0.56017(13) 0.0518(5) Uani 1 1 d . . . . .
C6 C 0.3358(2) 0.3525(2) 0.62806(12) 0.0460(5) Uani 1 1 d . . . . .
H6 H 0.4211 0.4103 0.6142 0.055 Uiso 1 1 calc R U . . .
C7 C 0.3812(2) 0.2293(2) 0.64680(13) 0.0482(5) Uani 1 1 d . . . . .
C8 C 0.3136(2) 0.1720(2) 0.69822(13) 0.0509(5) Uani 1 1 d . . . . .
H8 H 0.3351 0.0922 0.7073 0.061 Uiso 1 1 calc R U . . .
C9 C 0.2087(2) 0.2295(2) 0.74006(13) 0.0484(5) Uani 1 1 d . . . . .
C10 C 0.2103(2) 0.3644(2) 0.74349(12) 0.0434(5) Uani 1 1 d . . . . .
C11 C 0.1124(3) 0.1505(2) 0.78317(14) 0.0575(6) Uani 1 1 d . . . . .
C12 C 0.0830(4) -0.0365(3) 0.84164(19) 0.0952(10) Uani 1 1 d . . . . .
H12A H 0.1304 -0.1081 0.8482 0.143 Uiso 1 1 calc R U . . .
H12B H 0.0788 0.0196 0.8916 0.143 Uiso 1 1 calc R U . . .
H12C H -0.0149 -0.0758 0.8148 0.143 Uiso 1 1 calc R U . . .
C13 C 0.5025(3) 0.1782(3) 0.61392(15) 0.0622(6) Uani 1 1 d . . . . .
C14 C 0.6935(4) 0.2173(4) 0.5375(2) 0.1177(13) Uani 1 1 d . . . . .
H14A H 0.7281 0.2749 0.5042 0.177 Uiso 1 1 calc R U . . .
H14B H 0.7687 0.2307 0.5805 0.177 Uiso 1 1 calc R U . . .
H14C H 0.6702 0.1234 0.5089 0.177 Uiso 1 1 calc R U . . .
C15 C 0.1323(2) 0.4489(2) 0.79577(12) 0.0438(5) Uani 1 1 d . . . . .
C16 C 0.1556(2) 0.4693(2) 0.87542(13) 0.0544(6) Uani 1 1 d . . . . .
H16 H 0.2199 0.4263 0.8977 0.065 Uiso 1 1 calc R U . . .
C17 C 0.0852(3) 0.5523(3) 0.92234(14) 0.0603(6) Uani 1 1 d . . . . .
H17 H 0.1022 0.5660 0.9760 0.072 Uiso 1 1 calc R U . . .
C18 C -0.0106(3) 0.6148(2) 0.88898(15) 0.0585(6) Uani 1 1 d . . . . .
C19 C -0.0373(3) 0.5951(2) 0.80976(14) 0.0551(6) Uani 1 1 d . . . . .
H19 H -0.1036 0.6366 0.7878 0.066 Uiso 1 1 calc R U . . .
C20 C 0.0351(2) 0.5134(2) 0.76338(13) 0.0491(5) Uani 1 1 d . . . . .
H20 H 0.0189 0.5011 0.7098 0.059 Uiso 1 1 calc R U . . .
C21 C 0.3520(2) 0.5751(2) 0.71956(12) 0.0458(5) Uani 1 1 d . . . . .
C22 C 0.4545(2) 0.6326(2) 0.78452(13) 0.0517(5) Uani 1 1 d . . . . .
C23 C 0.5166(3) 0.7712(3) 0.80556(16) 0.0705(7) Uani 1 1 d . . . . .
H23 H 0.5853 0.8094 0.8499 0.085 Uiso 1 1 calc R U . . .
C24 C 0.4746(4) 0.8520(3) 0.75928(19) 0.0796(8) Uani 1 1 d . . . . .
H24 H 0.5148 0.9457 0.7729 0.096 Uiso 1 1 calc R U . . .
C25 C 0.3752(3) 0.7961(3) 0.69397(17) 0.0727(8) Uani 1 1 d . . . . .
H25 H 0.3491 0.8514 0.6629 0.087 Uiso 1 1 calc R U . . .
C26 C 0.3128(3) 0.6576(2) 0.67363(14) 0.0590(6) Uani 1 1 d . . . . .
H26 H 0.2445 0.6198 0.6291 0.071 Uiso 1 1 calc R U . . .
C27 C 0.5825(2) 0.4671(2) 0.80386(14) 0.0556(6) Uani 1 1 d . . . . .
C28 C 0.6049(2) 0.3723(2) 0.85345(13) 0.0537(6) Uani 1 1 d . . . . .
C29 C 0.5323(3) 0.3639(3) 0.91678(15) 0.0688(7) Uani 1 1 d . . . . .
H29 H 0.4681 0.4200 0.9299 0.083 Uiso 1 1 calc R U . . .
C30 C 0.5539(3) 0.2732(3) 0.96098(15) 0.0730(7) Uani 1 1 d . . . . .
H30 H 0.5053 0.2675 1.0038 0.088 Uiso 1 1 calc R U . . .
C31 C 0.6490(3) 0.1919(3) 0.93987(14) 0.0586(6) Uani 1 1 d . . . . .
C32 C 0.7233(3) 0.1988(3) 0.87825(15) 0.0642(7) Uani 1 1 d . . . . .
H32 H 0.7879 0.1428 0.8657 0.077 Uiso 1 1 calc R U . . .
C33 C 0.7013(3) 0.2905(3) 0.83429(15) 0.0626(6) Uani 1 1 d . . . . .
H33 H 0.7514 0.2966 0.7921 0.075 Uiso 1 1 calc R U . . .
N1 N 0.2401(3) 0.2546(3) 0.49252(12) 0.0719(7) Uani 1 1 d . . . . .
N2 N 0.29305(18) 0.43044(16) 0.69775(10) 0.0442(4) Uani 1 1 d . . . . .
N3 N 0.6757(3) 0.0964(2) 0.98770(14) 0.0728(6) Uani 1 1 d . . . . .
O1 O 0.0912(2) 0.3427(2) 0.56978(11) 0.0896(7) Uani 1 1 d . . . . .
O2 O 0.5444(2) 0.0819(2) 0.62678(14) 0.1009(8) Uani 1 1 d . . . . .
O3 O 0.5624(2) 0.25179(19) 0.56630(11) 0.0747(5) Uani 1 1 d . . . . .
O4 O -0.0001(2) 0.1713(2) 0.80309(14) 0.0919(7) Uani 1 1 d . . . . .
O5 O 0.1657(2) 0.04620(18) 0.79695(11) 0.0758(5) Uani 1 1 d . . . . .
O6 O 0.49399(17) 0.54985(16) 0.83245(9) 0.0590(4) Uani 1 1 d . . . . .
O7 O 0.63425(19) 0.47127(19) 0.74493(10) 0.0692(5) Uani 1 1 d . . . . .
O8 O 0.6302(3) 0.1090(3) 1.05037(14) 0.1092(8) Uani 1 1 d . . . . .
O9 O 0.7409(3) 0.0099(2) 0.96213(13) 0.0931(6) Uani 1 1 d . . . . .
Cl1 Cl -0.10151(10) 0.71899(8) 0.94750(5) 0.0976(3) Uani 1 1 d . . . . .
H1 H 0.321(3) 0.244(3) 0.4936(16) 0.071(9) 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
C1 C4 1.500(4) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C4 1.488(5) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 C4 1.509(5) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 N1 1.469(3) . ?
C5 O1 1.210(3) . ?
C5 N1 1.323(3) . ?
C5 C6 1.547(3) . ?
C6 N2 1.463(3) . ?
C6 C7 1.514(3) . ?
C6 H6 0.9800 . ?
C7 C8 1.333(3) . ?
C7 C13 1.467(3) . ?
C8 C9 1.436(3) . ?
C8 H8 0.9300 . ?
C9 C10 1.376(3) . ?
C9 C11 1.471(3) . ?
C10 N2 1.367(3) . ?
C10 C15 1.483(3) . ?
C11 O4 1.190(3) . ?
C11 O5 1.337(3) . ?
C12 O5 1.449(3) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 O2 1.200(3) . ?
C13 O3 1.343(3) . ?
C14 O3 1.457(3) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 C16 1.380(3) . ?
C15 C20 1.391(3) . ?
C16 C17 1.376(3) . ?
C16 H16 0.9300 . ?
C17 C18 1.375(4) . ?
C17 H17 0.9300 . ?
C18 C19 1.375(3) . ?
C18 Cl1 1.739(2) . ?
C19 C20 1.375(3) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
C21 C22 1.373(3) . ?
C21 C26 1.382(3) . ?
C21 N2 1.432(3) . ?
C22 C23 1.380(3) . ?
C22 O6 1.411(3) . ?
C23 C24 1.382(4) . ?
C23 H23 0.9300 . ?
C24 C25 1.361(4) . ?
C24 H24 0.9300 . ?
C25 C26 1.379(4) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C27 O7 1.202(3) . ?
C27 O6 1.364(3) . ?
C27 C28 1.487(3) . ?
C28 C33 1.377(3) . ?
C28 C29 1.380(3) . ?
C29 C30 1.382(4) . ?
C29 H29 0.9300 . ?
C30 C31 1.369(4) . ?
C30 H30 0.9300 . ?
C31 C32 1.360(3) . ?
C31 N3 1.481(3) . ?
C32 C33 1.388(4) . ?
C32 H32 0.9300 . ?
C33 H33 0.9300 . ?
N1 H1 0.79(3) . ?
N3 O9 1.215(3) . ?
N3 O8 1.222(3) . ?

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
C4 C1 H1A 109.5 . . ?
C4 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C4 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C4 C2 H2A 109.5 . . ?
C4 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C4 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C3 H3A 109.5 . . ?
C4 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C4 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N1 C4 C2 109.6(3) . . ?
N1 C4 C1 107.3(2) . . ?
C2 C4 C1 112.1(4) . . ?
N1 C4 C3 109.9(3) . . ?
C2 C4 C3 107.6(4) . . ?
C1 C4 C3 110.4(3) . . ?
O1 C5 N1 124.1(2) . . ?
O1 C5 C6 121.3(2) . . ?
N1 C5 C6 114.51(19) . . ?
N2 C6 C7 108.53(16) . . ?
N2 C6 C5 109.57(16) . . ?
C7 C6 C5 113.60(17) . . ?
N2 C6 H6 108.3 . . ?
C7 C6 H6 108.3 . . ?
C5 C6 H6 108.3 . . ?
C8 C7 C13 120.0(2) . . ?
C8 C7 C6 118.15(19) . . ?
C13 C7 C6 121.8(2) . . ?
C7 C8 C9 122.13(19) . . ?
C7 C8 H8 118.9 . . ?
C9 C8 H8 118.9 . . ?
C10 C9 C8 117.39(19) . . ?
C10 C9 C11 121.4(2) . . ?
C8 C9 C11 121.02(19) . . ?
N2 C10 C9 119.18(19) . . ?
N2 C10 C15 115.60(16) . . ?
C9 C10 C15 125.18(18) . . ?
O4 C11 O5 122.4(2) . . ?
O4 C11 C9 126.6(2) . . ?
O5 C11 C9 111.0(2) . . ?
O5 C12 H12A 109.5 . . ?
O5 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
O5 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O2 C13 O3 123.0(2) . . ?
O2 C13 C7 125.1(2) . . ?
O3 C13 C7 112.0(2) . . ?
O3 C14 H14A 109.5 . . ?
O3 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
O3 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 C20 118.8(2) . . ?
C16 C15 C10 122.56(18) . . ?
C20 C15 C10 118.65(18) . . ?
C17 C16 C15 121.0(2) . . ?
C17 C16 H16 119.5 . . ?
C15 C16 H16 119.5 . . ?
C18 C17 C16 119.2(2) . . ?
C18 C17 H17 120.4 . . ?
C16 C17 H17 120.4 . . ?
C19 C18 C17 121.1(2) . . ?
C19 C18 Cl1 119.2(2) . . ?
C17 C18 Cl1 119.7(2) . . ?
C18 C19 C20 119.3(2) . . ?
C18 C19 H19 120.3 . . ?
C20 C19 H19 120.3 . . ?
C19 C20 C15 120.7(2) . . ?
C19 C20 H20 119.7 . . ?
C15 C20 H20 119.7 . . ?
C22 C21 C26 119.1(2) . . ?
C22 C21 N2 120.05(18) . . ?
C26 C21 N2 120.7(2) . . ?
C21 C22 C23 121.3(2) . . ?
C21 C22 O6 119.69(19) . . ?
C23 C22 O6 119.0(2) . . ?
C22 C23 C24 118.6(3) . . ?
C22 C23 H23 120.7 . . ?
C24 C23 H23 120.7 . . ?
C25 C24 C23 120.7(2) . . ?
C25 C24 H24 119.6 . . ?
C23 C24 H24 119.6 . . ?
C24 C25 C26 120.3(2) . . ?
C24 C25 H25 119.8 . . ?
C26 C25 H25 119.8 . . ?
C25 C26 C21 119.9(2) . . ?
C25 C26 H26 120.0 . . ?
C21 C26 H26 120.0 . . ?
O7 C27 O6 122.9(2) . . ?
O7 C27 C28 124.9(2) . . ?
O6 C27 C28 112.1(2) . . ?
C33 C28 C29 119.8(2) . . ?
C33 C28 C27 117.9(2) . . ?
C29 C28 C27 122.3(2) . . ?
C28 C29 C30 120.8(2) . . ?
C28 C29 H29 119.6 . . ?
C30 C29 H29 119.6 . . ?
C31 C30 C29 118.0(2) . . ?
C31 C30 H30 121.0 . . ?
C29 C30 H30 121.0 . . ?
C32 C31 C30 122.6(2) . . ?
C32 C31 N3 118.8(2) . . ?
C30 C31 N3 118.6(2) . . ?
C31 C32 C33 119.1(2) . . ?
C31 C32 H32 120.5 . . ?
C33 C32 H32 120.5 . . ?
C28 C33 C32 119.7(2) . . ?
C28 C33 H33 120.1 . . ?
C32 C33 H33 120.1 . . ?
C5 N1 C4 128.4(2) . . ?
C5 N1 H1 115(2) . . ?
C4 N1 H1 117(2) . . ?
C10 N2 C21 121.77(17) . . ?
C10 N2 C6 120.32(16) . . ?
C21 N2 C6 117.66(16) . . ?
O9 N3 O8 124.0(2) . . ?
O9 N3 C31 118.1(2) . . ?
O8 N3 C31 117.9(2) . . ?
C13 O3 C14 115.6(2) . . ?
C11 O5 C12 116.2(2) . . ?
C27 O6 C22 115.62(17) . . ?

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
O1 C5 C6 N2 -4.7(3) . . . . ?
N1 C5 C6 N2 174.7(2) . . . . ?
O1 C5 C6 C7 116.9(3) . . . . ?
N1 C5 C6 C7 -63.7(3) . . . . ?
N2 C6 C7 C8 32.7(3) . . . . ?
C5 C6 C7 C8 -89.5(2) . . . . ?
N2 C6 C7 C13 -143.3(2) . . . . ?
C5 C6 C7 C13 94.6(2) . . . . ?
C13 C7 C8 C9 171.2(2) . . . . ?
C6 C7 C8 C9 -4.8(3) . . . . ?
C7 C8 C9 C10 -18.7(3) . . . . ?
C7 C8 C9 C11 166.5(2) . . . . ?
C8 C9 C10 N2 10.3(3) . . . . ?
C11 C9 C10 N2 -174.97(19) . . . . ?
C8 C9 C10 C15 -167.40(19) . . . . ?
C11 C9 C10 C15 7.4(3) . . . . ?
C10 C9 C11 O4 25.6(4) . . . . ?
C8 C9 C11 O4 -159.8(3) . . . . ?
C10 C9 C11 O5 -155.7(2) . . . . ?
C8 C9 C11 O5 18.9(3) . . . . ?
C8 C7 C13 O2 3.6(4) . . . . ?
C6 C7 C13 O2 179.5(2) . . . . ?
C8 C7 C13 O3 -176.9(2) . . . . ?
C6 C7 C13 O3 -1.0(3) . . . . ?
N2 C10 C15 C16 -120.5(2) . . . . ?
C9 C10 C15 C16 57.3(3) . . . . ?
N2 C10 C15 C20 57.6(3) . . . . ?
C9 C10 C15 C20 -124.7(2) . . . . ?
C20 C15 C16 C17 -0.4(3) . . . . ?
C10 C15 C16 C17 177.6(2) . . . . ?
C15 C16 C17 C18 0.5(3) . . . . ?
C16 C17 C18 C19 0.3(4) . . . . ?
C16 C17 C18 Cl1 179.49(17) . . . . ?
C17 C18 C19 C20 -1.2(3) . . . . ?
Cl1 C18 C19 C20 179.65(17) . . . . ?
C18 C19 C20 C15 1.2(3) . . . . ?
C16 C15 C20 C19 -0.5(3) . . . . ?
C10 C15 C20 C19 -178.60(19) . . . . ?
C26 C21 C22 C23 1.3(3) . . . . ?
N2 C21 C22 C23 177.9(2) . . . . ?
C26 C21 C22 O6 179.17(19) . . . . ?
N2 C21 C22 O6 -4.2(3) . . . . ?
C21 C22 C23 C24 -0.6(4) . . . . ?
O6 C22 C23 C24 -178.5(2) . . . . ?
C22 C23 C24 C25 -0.6(4) . . . . ?
C23 C24 C25 C26 1.1(4) . . . . ?
C24 C25 C26 C21 -0.3(4) . . . . ?
C22 C21 C26 C25 -0.8(3) . . . . ?
N2 C21 C26 C25 -177.4(2) . . . . ?
O7 C27 C28 C33 5.5(4) . . . . ?
O6 C27 C28 C33 -175.1(2) . . . . ?
O7 C27 C28 C29 -174.2(2) . . . . ?
O6 C27 C28 C29 5.2(3) . . . . ?
C33 C28 C29 C30 -0.7(4) . . . . ?
C27 C28 C29 C30 179.0(2) . . . . ?
C28 C29 C30 C31 -0.2(4) . . . . ?
C29 C30 C31 C32 0.8(4) . . . . ?
C29 C30 C31 N3 178.7(2) . . . . ?
C30 C31 C32 C33 -0.7(4) . . . . ?
N3 C31 C32 C33 -178.5(2) . . . . ?
C29 C28 C33 C32 0.8(4) . . . . ?
C27 C28 C33 C32 -178.8(2) . . . . ?
C31 C32 C33 C28 -0.2(4) . . . . ?
O1 C5 N1 C4 2.7(5) . . . . ?
C6 C5 N1 C4 -176.7(3) . . . . ?
C2 C4 N1 C5 -62.1(4) . . . . ?
C1 C4 N1 C5 176.0(4) . . . . ?
C3 C4 N1 C5 56.0(4) . . . . ?
C9 C10 N2 C21 -152.4(2) . . . . ?
C15 C10 N2 C21 25.5(3) . . . . ?
C9 C10 N2 C6 21.7(3) . . . . ?
C15 C10 N2 C6 -160.41(17) . . . . ?
C22 C21 N2 C10 64.4(3) . . . . ?
C26 C21 N2 C10 -119.0(2) . . . . ?
C22 C21 N2 C6 -109.9(2) . . . . ?
C26 C21 N2 C6 66.7(3) . . . . ?
C7 C6 N2 C10 -41.9(2) . . . . ?
C5 C6 N2 C10 82.7(2) . . . . ?
C7 C6 N2 C21 132.47(18) . . . . ?
C5 C6 N2 C21 -103.0(2) . . . . ?
C32 C31 N3 O9 -13.6(4) . . . . ?
C30 C31 N3 O9 168.5(3) . . . . ?
C32 C31 N3 O8 166.7(3) . . . . ?
C30 C31 N3 O8 -11.2(4) . . . . ?
O2 C13 O3 C14 -6.7(4) . . . . ?
C7 C13 O3 C14 173.8(3) . . . . ?
O4 C11 O5 C12 -3.4(4) . . . . ?
C9 C11 O5 C12 177.8(2) . . . . ?
O7 C27 O6 C22 5.9(3) . . . . ?
C28 C27 O6 C22 -173.46(18) . . . . ?
C21 C22 O6 C27 74.6(3) . . . . ?
C23 C22 O6 C27 -107.5(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
C2 H2C O1 0.96 2.52 3.110(5) 119.8 .
C3 H3B O1 0.96 2.47 3.067(4) 120.1 .
C19 H19 O7 0.93 2.63 3.093(3) 111.6 1_455
C23 H23 O9 0.93 2.61 3.478(4) 154.6 1_565
C32 H32 O4 0.93 2.37 3.065(3) 131.7 1_655
N1 H1 O3 0.79(3) 2.49(3) 3.199(3) 151(3) .

_refine_diff_density_max         0.349
_refine_diff_density_min         -0.232
_refine_diff_density_rms         0.068

# start Validation Reply Form
_vrf_PLAT242_JR637               
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of         C4 Check 
RESPONSE: The atom belongs to terminal t-butyl group
;
_vrf_PLAT910_JR637               
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         12 Note  
RESPONSE: The intensity of these reflections are cut by beamstop.
;
# end Validation Reply Form


