####################################################################### 
# 
# 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_Comp38_a
_database_code_depnum_ccdc_archive 'CCDC 1938950'
loop_
_audit_author_name
_audit_author_address
'Abdur Rahim'
;Shiv Nadar University
India
;
_audit_update_record             
;
2019-12-31 deposited with the CCDC.	2019-12-31 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT035_Comp38_a            
;
PROBLEM: _chemical_absolute_configuration Info  Not Given     Please Do !
RESPONSE: Manual inspection did not show any error
;
# Added during the CSD deposition process: Tuesday 31 December 2019 04:38 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
(S)-4-methoxy-N-(3-methyl-2,5-dioxopiperazin-1-yl)benzamide
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C13 H15 N3 O4,H2 O'
_chemical_formula_sum            'C13 H17 N3 O5'
_chemical_formula_weight         295.30

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      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   5.8031(6)
_cell_length_b                   11.3443(9)
_cell_length_c                   22.168(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1459.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    2136
_cell_measurement_theta_min      2.02
_cell_measurement_theta_max      26.37

_exptl_crystal_description       SLAB
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_F_000             634
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.145
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.048
_exptl_absorpt_coefficient_mu    0.105
_shelx_estimated_absorpt_T_min   0.982
_shelx_estimated_absorpt_T_max   0.994
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.871
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   X-ray
_diffrn_measurement_device_type  'Bruker PHOTON100 CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            3729
_diffrn_reflns_av_unetI/netI     0.0705
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.017
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_full        25.242
_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 0.922
_diffrn_reflns_point_group_measured_fraction_full 0.930
_reflns_number_total             2983
_reflns_number_gt                1791
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.570
_reflns_Friedel_fraction_max     0.812
_reflns_Friedel_fraction_full    0.830

_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-2014/7 (Sheldrick, 2014)'
_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)+(0.1000P)²+0.2155P] 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       0.015(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 470 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -2.5(10)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2752
_refine_ls_number_parameters     209
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0933
_refine_ls_R_factor_gt           0.0548
_refine_ls_wR_factor_ref         0.1728
_refine_ls_wR_factor_gt          0.1391
_refine_ls_goodness_of_fit_ref   0.885
_refine_ls_restrained_S_all      0.885
_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
O2 O 0.2130(6) 0.5490(4) 0.40055(15) 0.0575(10) Uani 1 1 d . . . . .
N2 N 0.5597(7) 0.7018(4) 0.40950(17) 0.0454(10) Uani 1 1 d . . . . .
O1 O 0.0893(8) 0.2130(4) 0.62292(18) 0.0749(13) Uani 1 1 d . . . . .
O3 O 0.3012(8) 0.8306(4) 0.44495(19) 0.0774(14) Uani 1 1 d . . . . .
N1 N 0.5068(7) 0.6220(4) 0.4553(2) 0.0494(11) Uani 1 1 d . . . . .
N3 N 0.6694(8) 0.8453(4) 0.3144(2) 0.0599(13) Uani 1 1 d . . . . .
O5 O 0.2167(11) 0.5242(6) 0.2729(3) 0.0896(16) Uani 1 1 d . . . . .
O4 O 0.8904(8) 0.7048(5) 0.2721(2) 0.0904(16) Uani 1 1 d . . . . .
C4 C 0.2690(7) 0.4667(4) 0.49781(19) 0.0376(10) Uani 1 1 d . . . . .
C8 C 0.3240(8) 0.5483(4) 0.4478(2) 0.0402(11) Uani 1 1 d . . . . .
C5 C 0.4226(8) 0.4403(4) 0.5440(2) 0.0419(11) Uani 1 1 d . . . . .
H5 H 0.5635 0.4792 0.5458 0.050 Uiso 1 1 calc R U . . .
C9 C 0.4454(8) 0.8037(4) 0.4074(2) 0.0443(11) Uani 1 1 d . . . . .
C3 C 0.0587(7) 0.4085(4) 0.4962(2) 0.0436(11) Uani 1 1 d . . . . .
H3 H -0.0458 0.4254 0.4656 0.052 Uiso 1 1 calc R U . . .
C10 C 0.5058(9) 0.8893(4) 0.3585(2) 0.0469(12) Uani 1 1 d . . . . .
H10 H 0.5781 0.9573 0.3781 0.056 Uiso 1 1 calc R U . . .
C1 C 0.1574(9) 0.2994(5) 0.5846(2) 0.0481(12) Uani 1 1 d . . . . .
C6 C 0.3688(8) 0.3568(5) 0.5873(2) 0.0499(13) Uani 1 1 d . . . . .
H6 H 0.4729 0.3393 0.6180 0.060 Uiso 1 1 calc R U . . .
C2 C 0.0033(8) 0.3267(5) 0.5391(2) 0.0498(13) Uani 1 1 d . . . . .
H2 H -0.1391 0.2892 0.5377 0.060 Uiso 1 1 calc R U . . .
C11 C 0.7612(9) 0.7386(5) 0.3123(2) 0.0564(14) Uani 1 1 d . . . . .
C12 C 0.7106(9) 0.6562(5) 0.3631(3) 0.0625(16) Uani 1 1 d . . . . .
H12A H 0.6417 0.5853 0.3466 0.075 Uiso 1 1 calc R U . . .
H12B H 0.8554 0.6338 0.3817 0.075 Uiso 1 1 calc R U . . .
C13 C 0.2953(11) 0.9345(7) 0.3264(3) 0.086(2) Uani 1 1 d . . . . .
H13A H 0.3394 0.9949 0.2984 0.129 Uiso 1 1 calc R U . . .
H13B H 0.1892 0.9664 0.3553 0.129 Uiso 1 1 calc R U . . .
H13C H 0.2230 0.8709 0.3050 0.129 Uiso 1 1 calc R U . . .
C7 C 0.2317(16) 0.1869(7) 0.6726(3) 0.106(3) Uani 1 1 d . . . . .
H7A H 0.3799 0.1614 0.6584 0.159 Uiso 1 1 calc R U . . .
H7B H 0.1626 0.1253 0.6961 0.159 Uiso 1 1 calc R U . . .
H7C H 0.2497 0.2561 0.6970 0.159 Uiso 1 1 calc R U . . .
H1N H 0.587(11) 0.627(5) 0.487(3) 0.070(19) Uiso 1 1 d . . . . .
H3N H 0.707(13) 0.901(7) 0.281(3) 0.11(2) Uiso 1 1 d . . . . .
H1O H 0.233(18) 0.508(8) 0.310(5) 0.14(4) Uiso 1 1 d . . . . .
H2O H 0.108(14) 0.582(7) 0.275(3) 0.11(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
O2 C8 1.230(5) . ?
N2 C9 1.334(6) . ?
N2 N1 1.395(5) . ?
N2 C12 1.446(6) . ?
O1 C1 1.356(6) . ?
O1 C7 1.408(8) . ?
O3 C9 1.219(6) . ?
N1 C8 1.361(6) . ?
N1 H1N 0.85(6) . ?
N3 C11 1.323(7) . ?
N3 C10 1.451(7) . ?
N3 H3N 1.01(8) . ?
O5 H1O 0.86(10) . ?
O5 H2O 0.91(9) . ?
O4 C11 1.227(6) . ?
C4 C3 1.388(6) . ?
C4 C5 1.390(6) . ?
C4 C8 1.479(6) . ?
C5 C6 1.386(7) . ?
C5 H5 0.9300 . ?
C9 C10 1.498(6) . ?
C3 C2 1.367(7) . ?
C3 H3 0.9300 . ?
C10 C13 1.503(8) . ?
C10 H10 0.9800 . ?
C1 C2 1.383(7) . ?
C1 C6 1.390(7) . ?
C6 H6 0.9300 . ?
C2 H2 0.9300 . ?
C11 C12 1.493(7) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 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
C9 N2 N1 118.6(4) . . ?
C9 N2 C12 125.9(4) . . ?
N1 N2 C12 114.8(4) . . ?
C1 O1 C7 118.1(4) . . ?
C8 N1 N2 118.8(4) . . ?
C8 N1 H1N 125(4) . . ?
N2 N1 H1N 116(4) . . ?
C11 N3 C10 127.0(5) . . ?
C11 N3 H3N 117(4) . . ?
C10 N3 H3N 115(4) . . ?
H1O O5 H2O 101(8) . . ?
C3 C4 C5 118.8(4) . . ?
C3 C4 C8 117.9(4) . . ?
C5 C4 C8 123.2(4) . . ?
O2 C8 N1 120.5(5) . . ?
O2 C8 C4 122.0(4) . . ?
N1 C8 C4 117.5(4) . . ?
C6 C5 C4 120.9(4) . . ?
C6 C5 H5 119.6 . . ?
C4 C5 H5 119.6 . . ?
O3 C9 N2 122.4(5) . . ?
O3 C9 C10 119.5(5) . . ?
N2 C9 C10 118.1(4) . . ?
C2 C3 C4 120.7(4) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 H3 119.6 . . ?
N3 C10 C9 114.7(4) . . ?
N3 C10 C13 109.3(4) . . ?
C9 C10 C13 112.0(5) . . ?
N3 C10 H10 106.8 . . ?
C9 C10 H10 106.8 . . ?
C13 C10 H10 106.8 . . ?
O1 C1 C2 115.5(4) . . ?
O1 C1 C6 124.6(5) . . ?
C2 C1 C6 119.8(5) . . ?
C5 C6 C1 119.3(5) . . ?
C5 C6 H6 120.4 . . ?
C1 C6 H6 120.4 . . ?
C3 C2 C1 120.5(4) . . ?
C3 C2 H2 119.7 . . ?
C1 C2 H2 119.7 . . ?
O4 C11 N3 123.9(5) . . ?
O4 C11 C12 118.2(5) . . ?
N3 C11 C12 117.8(5) . . ?
N2 C12 C11 115.6(5) . . ?
N2 C12 H12A 108.4 . . ?
C11 C12 H12A 108.4 . . ?
N2 C12 H12B 108.4 . . ?
C11 C12 H12B 108.4 . . ?
H12A C12 H12B 107.4 . . ?
C10 C13 H13A 109.5 . . ?
C10 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C10 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O1 C7 H7A 109.5 . . ?
O1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
O1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?

_refine_diff_density_max         0.176
_refine_diff_density_min         -0.172
_refine_diff_density_rms         0.039



