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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
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#######################################################################

data_29novb_a
_database_code_depnum_ccdc_archive 'CCDC 2329775'
loop_
_audit_author_name
_audit_author_address
'Dr. Subrata Das'
;Associate Professor, Dept of Chemistry, NIT Patna
India
;
_audit_update_record             
;
2024-10-03 deposited with the CCDC.	2024-10-23 downloaded from the CCDC.
;
_audit_creation_date             2024-10-02
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C4 H4 Br Cl N4, C4 H5 N O2'
_chemical_formula_sum            'C8 H9 Br Cl N5 O2'
_chemical_formula_weight         322.56
_chemical_melting_point          ?
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'
Br Br -0.2901 2.4595 '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'
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   7.7958(4)
_cell_length_b                   6.4753(3)
_cell_length_c                   22.4577(12)
_cell_angle_alpha                90
_cell_angle_beta                 90.521(2)
_cell_angle_gamma                90
_cell_volume                     1133.62(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9892
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      28.39
_cell_measurement_theta_min      2.76
_shelx_estimated_absorpt_T_max   0.676
_shelx_estimated_absorpt_T_min   0.458
_exptl_absorpt_coefficient_mu    3.860
_exptl_absorpt_correction_T_max  0.4666
_exptl_absorpt_correction_T_min  0.3544
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_factor_muR        1.004
_exptl_absorpt_process_details   
;
Walker, N. & Stuart, D (1983) Acta. Cryst. A39, 158-166
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.890
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0633
_diffrn_reflns_av_unetI/netI     0.0398
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            2070
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.774
_diffrn_ambient_temperature      273.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'Bruker diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2033
_reflns_number_total             2070
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_refine_diff_density_max         0.692
_refine_diff_density_min         -0.709
_refine_diff_density_rms         0.207
_refine_ls_extinction_coef       0.026(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         2070
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0376
_refine_ls_restrained_S_all      1.156
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0637P)²+1.0654P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1051
_refine_ls_wR_factor_ref         0.1056
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups, All N(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C6(H6A,H6B)
2.b Aromatic/amide H refined with riding coordinates:
 N5(H5)
2.c X=CH2 refined with riding coordinates:
 N3(H3A,H3B), N4(H4A,H4B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Br1 Br 0.31460(4) 0.70811(5) 0.34149(2) 0.0157(2) Uani 1 1 d . . . . .
Cl1 Cl 0.50969(9) 0.25747(12) 0.34284(3) 0.0153(2) Uani 1 1 d . . . . .
O1 O -0.0113(3) 0.8712(3) 0.58379(9) 0.0147(5) Uani 1 1 d . . . . .
O2 O 0.1898(3) 0.2883(3) 0.67302(12) 0.0179(5) Uani 1 1 d . . . . .
N1 N 0.4199(3) 0.2147(4) 0.45301(12) 0.0116(5) Uani 1 1 d . . . . .
N2 N 0.2480(3) 0.4549(4) 0.50791(10) 0.0107(5) Uani 1 1 d . . . . .
N3 N 0.3451(3) 0.1518(4) 0.54981(11) 0.0142(5) Uani 1 1 d . . . . .
H3A H 0.294234 0.185210 0.582233 0.017 Uiso 1 1 calc R U . . .
H3B H 0.401034 0.037562 0.547747 0.017 Uiso 1 1 calc R U . . .
N4 N 0.1539(3) 0.7583(4) 0.46652(12) 0.0133(5) Uani 1 1 d . . . . .
H4A H 0.104208 0.787246 0.499519 0.016 Uiso 1 1 calc R U . . .
H4B H 0.147381 0.842933 0.437070 0.016 Uiso 1 1 calc R U . . .
C1 C 0.4093(3) 0.3428(5) 0.40719(13) 0.0106(5) Uani 1 1 d . . . . .
N5 N 0.0983(3) 0.5645(4) 0.61730(10) 0.0110(5) Uani 1 1 d . . . . .
H5 H 0.127820 0.516691 0.583161 0.013 Uiso 1 1 calc R U . . .
C2 C 0.3236(3) 0.5287(4) 0.40706(12) 0.0100(5) Uani 1 1 d . . . . .
C4 C 0.3372(4) 0.2774(4) 0.50260(14) 0.0102(6) Uani 1 1 d . . . . .
C5 C 0.0216(4) 0.7538(5) 0.62442(14) 0.0107(6) Uani 1 1 d . . . . .
C3 C 0.2405(3) 0.5832(4) 0.46104(12) 0.0100(6) Uani 1 1 d . . . . .
C8 C 0.1238(3) 0.4581(5) 0.66982(13) 0.0130(6) Uani 1 1 d . . . . .
C7 C 0.0559(4) 0.5888(5) 0.71992(12) 0.0150(6) Uani 1 1 d . . . . .
H7A H 0.146539 0.621350 0.748287 0.018 Uiso 1 1 calc R U . . .
H7B H -0.035362 0.517531 0.740584 0.018 Uiso 1 1 calc R U . . .
C6 C -0.0120(4) 0.7857(5) 0.69005(14) 0.0154(7) Uani 1 1 d . . . . .
H6A H -0.133624 0.802733 0.697259 0.019 Uiso 1 1 calc R U . . .
H6B H 0.048492 0.906440 0.704841 0.019 Uiso 1 1 calc R U . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Br1 0.0205(3) 0.0165(3) 0.0101(2) 0.00417(10) 0.00302(14) -0.00001(10)
Cl1 0.0152(4) 0.0177(4) 0.0130(4) -0.0039(3) 0.0068(3) 0.0002(3)
O1 0.0181(10) 0.0133(11) 0.0127(10) 0.0019(9) 0.0018(8) 0.0036(8)
O2 0.0216(13) 0.0177(13) 0.0144(12) 0.0027(8) -0.0019(9) 0.0041(8)
N1 0.0096(12) 0.0132(13) 0.0119(13) -0.0008(9) 0.0011(10) -0.0003(9)
N2 0.0121(11) 0.0110(11) 0.0089(11) 0.0005(9) 0.0012(9) 0.0020(9)
N3 0.0204(12) 0.0104(11) 0.0120(12) 0.0019(10) 0.0026(10) 0.0066(10)
N4 0.0193(13) 0.0116(11) 0.0091(13) 0.0016(10) 0.0039(10) 0.0047(10)
C1 0.0086(12) 0.0143(13) 0.0090(13) -0.0042(12) 0.0024(10) -0.0026(11)
N5 0.0133(11) 0.0132(12) 0.0064(11) -0.0008(9) 0.0011(9) 0.0025(9)
C2 0.0114(12) 0.0117(13) 0.0068(13) 0.0027(11) 0.0019(10) -0.0006(10)
C4 0.0074(13) 0.0118(14) 0.0115(16) -0.0023(11) 0.0008(11) -0.0029(10)
C5 0.0094(13) 0.0122(12) 0.0106(15) -0.0011(12) 0.0004(11) -0.0003(11)
C3 0.0092(12) 0.0105(13) 0.0105(13) 0.0001(11) -0.0002(10) -0.0026(10)
C8 0.0102(12) 0.0167(15) 0.0121(13) 0.0019(11) -0.0027(10) -0.0015(11)
C7 0.0204(14) 0.0173(14) 0.0074(13) 0.0004(12) -0.0005(11) -0.0009(12)
C6 0.0208(16) 0.0154(17) 0.0102(16) -0.0022(11) 0.0022(13) 0.0014(11)

_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
Br1 C2 1.876(3) . ?
Cl1 C1 1.740(3) . ?
O1 C5 1.213(4) . ?
O2 C8 1.216(4) . ?
N1 C1 1.324(4) . ?
N1 C4 1.354(4) . ?
N2 C4 1.349(4) . ?
N2 C3 1.342(4) . ?
N3 H3A 0.8600 . ?
N3 H3B 0.8600 . ?
N3 C4 1.337(4) . ?
N4 H4A 0.8600 . ?
N4 H4B 0.8600 . ?
N4 C3 1.326(4) . ?
C1 C2 1.377(4) . ?
N5 H5 0.8600 . ?
N5 C5 1.374(4) . ?
N5 C8 1.379(4) . ?
C2 C3 1.424(4) . ?
C5 C6 1.513(4) . ?
C8 C7 1.508(4) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C6 1.532(4) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?

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
C1 N1 C4 115.1(2) . . ?
C3 N2 C4 118.5(2) . . ?
H3A N3 H3B 120.0 . . ?
C4 N3 H3A 120.0 . . ?
C4 N3 H3B 120.0 . . ?
H4A N4 H4B 120.0 . . ?
C3 N4 H4A 120.0 . . ?
C3 N4 H4B 120.0 . . ?
N1 C1 Cl1 114.9(2) . . ?
N1 C1 C2 125.2(3) . . ?
C2 C1 Cl1 119.9(2) . . ?
C5 N5 H5 123.0 . . ?
C5 N5 C8 113.9(2) . . ?
C8 N5 H5 123.0 . . ?
C1 C2 Br1 123.9(2) . . ?
C1 C2 C3 116.1(2) . . ?
C3 C2 Br1 120.0(2) . . ?
N2 C4 N1 125.3(3) . . ?
N3 C4 N1 116.8(3) . . ?
N3 C4 N2 117.9(3) . . ?
O1 C5 N5 124.1(3) . . ?
O1 C5 C6 127.6(3) . . ?
N5 C5 C6 108.3(2) . . ?
N2 C3 C2 119.8(2) . . ?
N4 C3 N2 118.4(3) . . ?
N4 C3 C2 121.8(3) . . ?
O2 C8 N5 124.1(3) . . ?
O2 C8 C7 127.9(3) . . ?
N5 C8 C7 108.0(2) . . ?
C8 C7 H7A 110.7 . . ?
C8 C7 H7B 110.7 . . ?
C8 C7 C6 105.2(2) . . ?
H7A C7 H7B 108.8 . . ?
C6 C7 H7A 110.7 . . ?
C6 C7 H7B 110.7 . . ?
C5 C6 C7 104.5(2) . . ?
C5 C6 H6A 110.8 . . ?
C5 C6 H6B 110.8 . . ?
C7 C6 H6A 110.8 . . ?
C7 C6 H6B 110.8 . . ?
H6A C6 H6B 108.9 . . ?

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
Br1 C2 C3 N2 -179.69(19) . . . . ?
Br1 C2 C3 N4 0.8(4) . . . . ?
Cl1 C1 C2 Br1 -2.8(3) . . . . ?
Cl1 C1 C2 C3 178.0(2) . . . . ?
O1 C5 C6 C7 -179.9(3) . . . . ?
O2 C8 C7 C6 179.9(3) . . . . ?
N1 C1 C2 Br1 178.9(2) . . . . ?
N1 C1 C2 C3 -0.2(4) . . . . ?
C1 N1 C4 N2 0.1(4) . . . . ?
C1 N1 C4 N3 180.0(2) . . . . ?
C1 C2 C3 N2 -0.5(4) . . . . ?
C1 C2 C3 N4 180.0(3) . . . . ?
N5 C5 C6 C7 0.0(3) . . . . ?
N5 C8 C7 C6 -0.2(3) . . . . ?
C4 N1 C1 Cl1 -177.9(2) . . . . ?
C4 N1 C1 C2 0.4(4) . . . . ?
C4 N2 C3 N4 -179.5(2) . . . . ?
C4 N2 C3 C2 1.0(4) . . . . ?
C5 N5 C8 O2 -179.9(3) . . . . ?
C5 N5 C8 C7 0.2(3) . . . . ?
C3 N2 C4 N1 -0.8(4) . . . . ?
C3 N2 C4 N3 179.3(3) . . . . ?
C8 N5 C5 O1 179.7(3) . . . . ?
C8 N5 C5 C6 -0.1(3) . . . . ?
C8 C7 C6 C5 0.1(3) . . . . ?

_shelx_res_file                  
;
TITL 29novb_a.res in P2(1)/n
    29novb_a.res
    created by SHELXL-2019/3 at 12:52:29 on 02-Oct-2024
REM Old TITL 29novb in P2(1)/n
REM SHELXT solution in P2(1)/n
REM R1 0.204, Rweak 0.008, Alpha 0.035, Orientation as input
REM Formula found by SHELXT: C12 N O3 Br
CELL 0.71073 7.7958 6.4753 22.4577 90 90.521 90
ZERR 4 0.0004 0.0003 0.0012 0 0.002 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H Br Cl N O
UNIT 32 36 4 4 20 8

L.S. 99
PLAN  1
SIZE 0.24 0.11 0.12
TEMP 0
CONF
BOND $H
LIST 4
MORE -1
fmap 2
acta 50
SHEL 10 0.83
REM <olex2.extras>
REM <HklSrc "%.\\difabs.hkl">
REM </olex2.extras>

WGHT    0.065700    1.293800
EXTI    0.025563
FVAR       1.04960
BR1   3    0.314598    0.708110    0.341488    11.00000    0.02046    0.01650 =
         0.01013    0.00417    0.00302   -0.00001
CL1   4    0.509689    0.257472    0.342839    11.00000    0.01516    0.01771 =
         0.01303   -0.00395    0.00677    0.00021
O1    6   -0.011263    0.871208    0.583785    11.00000    0.01807    0.01331 =
         0.01273    0.00191    0.00182    0.00364
O2    6    0.189832    0.288252    0.673018    11.00000    0.02163    0.01775 =
         0.01440    0.00267   -0.00191    0.00409
N1    5    0.419944    0.214725    0.453013    11.00000    0.00961    0.01323 =
         0.01186   -0.00080    0.00114   -0.00025
N2    5    0.247989    0.454859    0.507912    11.00000    0.01211    0.01097 =
         0.00893    0.00049    0.00120    0.00204
N3    5    0.345097    0.151773    0.549808    11.00000    0.02041    0.01039 =
         0.01198    0.00190    0.00258    0.00659
AFIX  93
H3A   2    0.294234    0.185210    0.582233    11.00000   -1.20000
H3B   2    0.401034    0.037562    0.547747    11.00000   -1.20000
AFIX   0
N4    5    0.153892    0.758311    0.466518    11.00000    0.01927    0.01160 =
         0.00907    0.00163    0.00390    0.00469
AFIX  93
H4A   2    0.104208    0.787246    0.499519    11.00000   -1.20000
H4B   2    0.147381    0.842933    0.437070    11.00000   -1.20000
AFIX   0
C1    1    0.409278    0.342753    0.407186    11.00000    0.00855    0.01434 =
         0.00904   -0.00416    0.00240   -0.00258
N5    5    0.098324    0.564486    0.617298    11.00000    0.01334    0.01319 =
         0.00636   -0.00079    0.00107    0.00247
AFIX  43
H5    2    0.127820    0.516691    0.583161    11.00000   -1.20000
AFIX   0
C2    1    0.323594    0.528705    0.407057    11.00000    0.01143    0.01175 =
         0.00684    0.00273    0.00193   -0.00057
C4    1    0.337208    0.277370    0.502596    11.00000    0.00744    0.01177 =
         0.01149   -0.00228    0.00085   -0.00290
C5    1    0.021576    0.753786    0.624420    11.00000    0.00939    0.01224 =
         0.01062   -0.00106    0.00043   -0.00031
C3    1    0.240524    0.583246    0.461043    11.00000    0.00915    0.01047 =
         0.01050    0.00009   -0.00018   -0.00263
C8    1    0.123792    0.458052    0.669817    11.00000    0.01016    0.01670 =
         0.01208    0.00187   -0.00266   -0.00146
C7    1    0.055921    0.588841    0.719925    11.00000    0.02038    0.01733 =
         0.00741    0.00038   -0.00051   -0.00095
AFIX  23
H7A   2    0.146539    0.621350    0.748287    11.00000   -1.20000
H7B   2   -0.035362    0.517531    0.740584    11.00000   -1.20000
AFIX   0
C6    1   -0.011951    0.785687    0.690051    11.00000    0.02078    0.01537 =
         0.01023   -0.00224    0.00224    0.00143
AFIX  23
H6A   2   -0.133624    0.802733    0.697259    11.00000   -1.20000
H6B   2    0.048492    0.906440    0.704841    11.00000   -1.20000
AFIX   0
HKLF 4




REM  29novb_a.res in P2(1)/n
REM wR2 = 0.1056, GooF = S = 1.156, Restrained GooF = 1.156 for all data
REM R1 = 0.0376 for 2033 Fo > 4sig(Fo) and 0.0381 for all 2070 data
REM 155 parameters refined using 0 restraints

END

WGHT      0.0660      1.2850

REM Highest difference peak  0.692,  deepest hole -0.709,  1-sigma level  0.207
Q1    1   0.0190  0.7775  0.5592  11.00000  0.05    0.69
;
_shelx_res_checksum              8837
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_cb_61_b
_database_code_depnum_ccdc_archive 'CCDC 2348542'
loop_
_audit_author_name
_audit_author_address
'Dr. Subrata Das'
;Associate Professor, Dept of Chemistry, NIT Patna
India
;
_audit_update_record             
;
2024-08-27 deposited with the CCDC.	2024-10-23 downloaded from the CCDC.
;
_audit_creation_date             2024-08-23
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C7 H8 Br Cl N2 O2'
_chemical_formula_sum            'C7 H8 Br Cl N2 O2'
_chemical_formula_weight         267.51
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H N O Br Cl'
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'
Br Br -0.2901 2.4595 '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'
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   4.6708(5)
_cell_length_b                   15.1340(10)
_cell_length_c                   13.5776(8)
_cell_angle_alpha                90
_cell_angle_beta                 92.765(7)
_cell_angle_gamma                90
_cell_volume                     958.65(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1574
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.0430
_cell_measurement_theta_min      3.0850
_shelx_estimated_absorpt_T_max   1.000
_shelx_estimated_absorpt_T_min   0.148
_exptl_absorpt_coefficient_mu    4.535
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.14781
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.69a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light colourless'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.854
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.085
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0468
_diffrn_reflns_av_unetI/netI     0.0705
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4077
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.347
_diffrn_reflns_theta_min         2.016
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0303
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -12.00  33.00   1.00   18.00    --   14.69  77.00  90.00   45
  2  ω     -9.00  54.00   1.00   18.00    --   14.69 -99.00 -30.00   63
  3  ω    -22.00  36.00   1.00   18.00    --  -16.64  19.00 150.00   58
  4  ω    -65.00  -2.00   1.00   18.00    --  -16.64 -57.00 -30.00   63
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0195026000
_diffrn_orient_matrix_UB_12      0.0463269000
_diffrn_orient_matrix_UB_13      0.0042654000
_diffrn_orient_matrix_UB_21      0.1502457000
_diffrn_orient_matrix_UB_22      -0.0056858000
_diffrn_orient_matrix_UB_23      -0.0019716000
_diffrn_orient_matrix_UB_31      -0.0114508000
_diffrn_orient_matrix_UB_32      0.0039796000
_diffrn_orient_matrix_UB_33      -0.0521507000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1241
_reflns_number_total             1759
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.567
_refine_diff_density_min         -0.650
_refine_diff_density_rms         0.125
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         1759
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0787
_refine_ls_R_factor_gt           0.0470
_refine_ls_restrained_S_all      1.004
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0465P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0944
_refine_ls_wR_factor_ref         0.1076
_refine_special_details          ?
_olex2_refinement_description    
;
1.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B)
1.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C5(H5A,H5B,H5C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Br1 Br 0.33104(13) 0.19914(4) 0.83116(4) 0.0466(2) Uani 1 1 d . . . . .
Cl1 Cl 0.7025(3) 0.07079(9) 0.69460(10) 0.0466(4) Uani 1 1 d . . . . .
O1 O 0.3933(8) 0.3846(2) 0.7481(2) 0.0485(10) Uani 1 1 d . . . . .
O2 O 1.0467(8) 0.3306(2) 0.5191(3) 0.0526(11) Uani 1 1 d . . . . .
N1 N 0.8737(9) 0.2127(2) 0.6013(3) 0.0323(10) Uani 1 1 d . . . . .
N2 N 0.7214(9) 0.3573(3) 0.6334(3) 0.0324(10) Uani 1 1 d . . . . .
C1 C 0.5455(10) 0.2375(3) 0.7266(3) 0.0277(11) Uani 1 1 d . . . . .
C2 C 0.5402(11) 0.3311(3) 0.7062(3) 0.0343(12) Uani 1 1 d . . . . .
C4 C 0.7045(10) 0.1828(3) 0.6742(3) 0.0290(12) Uani 1 1 d . . . . .
C3 C 0.8925(11) 0.3020(3) 0.5798(3) 0.0334(12) Uani 1 1 d . . . . .
C6 C 1.0417(11) 0.1532(3) 0.5390(3) 0.0391(13) Uani 1 1 d . . . . .
H6A H 1.113310 0.104009 0.578766 0.047 Uiso 1 1 calc R U . . .
H6B H 1.205655 0.185286 0.516143 0.047 Uiso 1 1 calc R U . . .
C7 C 0.8692(13) 0.1182(4) 0.4517(4) 0.0582(17) Uani 1 1 d . . . . .
H7A H 0.991799 0.085307 0.410315 0.087 Uiso 1 1 calc R U . . .
H7B H 0.784677 0.166556 0.414924 0.087 Uiso 1 1 calc R U . . .
H7C H 0.720666 0.080240 0.473785 0.087 Uiso 1 1 calc R U . . .
C5 C 0.7389(12) 0.4527(3) 0.6117(4) 0.0587(18) Uani 1 1 d . . . . .
H5A H 0.558368 0.480125 0.623292 0.088 Uiso 1 1 calc R U . . .
H5B H 0.783399 0.460825 0.544023 0.088 Uiso 1 1 calc R U . . .
H5C H 0.886396 0.479030 0.653745 0.088 Uiso 1 1 calc R U . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Br1 0.0565(4) 0.0454(4) 0.0396(4) -0.0001(3) 0.0204(3) -0.0072(3)
Cl1 0.0650(10) 0.0272(7) 0.0489(8) 0.0019(6) 0.0144(7) 0.0034(6)
O1 0.064(3) 0.036(2) 0.048(2) 0.0004(18) 0.0277(19) 0.0134(19)
O2 0.071(3) 0.044(2) 0.046(2) -0.0003(19) 0.035(2) -0.004(2)
N1 0.042(3) 0.029(2) 0.027(2) 0.0015(18) 0.0103(18) 0.0077(19)
N2 0.044(3) 0.024(2) 0.030(2) 0.0037(19) 0.0086(18) 0.0013(19)
C1 0.037(3) 0.026(3) 0.021(2) 0.003(2) 0.005(2) -0.003(2)
C2 0.050(4) 0.030(3) 0.023(3) -0.004(2) 0.000(2) 0.003(3)
C4 0.041(3) 0.021(3) 0.026(3) 0.003(2) 0.003(2) -0.003(2)
C3 0.043(3) 0.032(3) 0.025(3) 0.000(2) 0.009(2) 0.002(2)
C6 0.044(3) 0.039(3) 0.035(3) -0.006(3) 0.012(2) 0.012(3)
C7 0.079(5) 0.056(4) 0.041(3) -0.018(3) 0.011(3) 0.016(3)
C5 0.089(5) 0.028(3) 0.061(4) 0.007(3) 0.026(3) -0.001(3)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 C1 1.869(4) . ?
Cl1 C4 1.718(5) . ?
O1 C2 1.219(6) . ?
O2 C3 1.201(6) . ?
N1 C4 1.373(5) . ?
N1 C3 1.386(6) . ?
N1 C6 1.485(6) . ?
N2 C2 1.390(6) . ?
N2 C3 1.388(6) . ?
N2 C5 1.475(6) . ?
C1 C2 1.443(7) . ?
C1 C4 1.340(6) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C7 1.498(7) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 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
C4 N1 C3 121.2(4) . . ?
C4 N1 C6 123.3(4) . . ?
C3 N1 C6 115.5(4) . . ?
C2 N2 C5 117.5(4) . . ?
C3 N2 C2 125.9(4) . . ?
C3 N2 C5 116.6(4) . . ?
C2 C1 Br1 116.5(4) . . ?
C4 C1 Br1 122.9(4) . . ?
C4 C1 C2 120.6(4) . . ?
O1 C2 N2 121.2(5) . . ?
O1 C2 C1 124.5(5) . . ?
N2 C2 C1 114.3(4) . . ?
N1 C4 Cl1 116.7(4) . . ?
C1 C4 Cl1 121.1(4) . . ?
C1 C4 N1 122.2(4) . . ?
O2 C3 N1 122.9(5) . . ?
O2 C3 N2 121.4(5) . . ?
N1 C3 N2 115.7(4) . . ?
N1 C6 H6A 109.0 . . ?
N1 C6 H6B 109.0 . . ?
N1 C6 C7 112.7(4) . . ?
H6A C6 H6B 107.8 . . ?
C7 C6 H6A 109.0 . . ?
C7 C6 H6B 109.0 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N2 C5 H5A 109.5 . . ?
N2 C5 H5B 109.5 . . ?
N2 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 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
Br1 C1 C2 O1 -4.7(7) . . . . ?
Br1 C1 C2 N2 174.9(3) . . . . ?
Br1 C1 C4 Cl1 4.5(6) . . . . ?
Br1 C1 C4 N1 -176.2(3) . . . . ?
C2 N2 C3 O2 -178.8(5) . . . . ?
C2 N2 C3 N1 1.0(7) . . . . ?
C2 C1 C4 Cl1 -177.5(3) . . . . ?
C2 C1 C4 N1 1.7(7) . . . . ?
C4 N1 C3 O2 177.1(5) . . . . ?
C4 N1 C3 N2 -2.7(7) . . . . ?
C4 N1 C6 C7 85.2(6) . . . . ?
C4 C1 C2 O1 177.2(5) . . . . ?
C4 C1 C2 N2 -3.2(7) . . . . ?
C3 N1 C4 Cl1 -179.3(4) . . . . ?
C3 N1 C4 C1 1.4(7) . . . . ?
C3 N1 C6 C7 -93.4(5) . . . . ?
C3 N2 C2 O1 -178.5(5) . . . . ?
C3 N2 C2 C1 1.8(7) . . . . ?
C6 N1 C4 Cl1 2.2(6) . . . . ?
C6 N1 C4 C1 -177.2(4) . . . . ?
C6 N1 C3 O2 -4.3(7) . . . . ?
C6 N1 C3 N2 176.0(4) . . . . ?
C5 N2 C2 O1 2.6(7) . . . . ?
C5 N2 C2 C1 -177.0(4) . . . . ?
C5 N2 C3 O2 0.1(7) . . . . ?
C5 N2 C3 N1 179.9(4) . . . . ?

_shelx_res_file                  
;
TITL cb_61_b_a.res in P2(1)/c
    cb_61_b.res
    created by SHELXL-2018/3 at 16:46:49 on 15-Apr-2024
REM Old TITL CB_61_B in P2(1)/c
REM SHELXT solution in P2(1)/c
REM R1 0.191, Rweak 0.244, Alpha 0.047, Orientation as input
REM Formula found by SHELXT: C5 N2 O2 Cl Br
CELL 0.71073 4.67078 15.133998 13.577605 90 92.7649 90
ZERR 4 0.000457 0.001019 0.000842 0 0.0067 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H Br Cl N O
UNIT 28 32 4 4 8 8

L.S. 99
PLAN  5
CONF
BOND $H
MORE -1
fmap 2
acta 50
SHEL 20 0.83
REM <olex2.extras>
REM <HklSrc "%.\\CB_61_B.hkl">
REM </olex2.extras>

WGHT    0.046500
FVAR       3.48685
BR1   3    0.331037    0.199141    0.831160    11.00000    0.05650    0.04536 =
         0.03957   -0.00005    0.02045   -0.00715
CL1   4    0.702478    0.070791    0.694602    11.00000    0.06496    0.02725 =
         0.04885    0.00193    0.01438    0.00342
O1    6    0.393307    0.384567    0.748052    11.00000    0.06409    0.03616 =
         0.04755    0.00035    0.02773    0.01336
O2    6    1.046679    0.330593    0.519068    11.00000    0.07082    0.04428 =
         0.04573   -0.00028    0.03507   -0.00412
N1    5    0.873664    0.212710    0.601268    11.00000    0.04204    0.02851 =
         0.02719    0.00147    0.01031    0.00772
N2    5    0.721412    0.357337    0.633353    11.00000    0.04385    0.02386 =
         0.03027    0.00370    0.00865    0.00127
C1    1    0.545522    0.237549    0.726610    11.00000    0.03663    0.02584 =
         0.02098    0.00275    0.00549   -0.00261
C2    1    0.540188    0.331111    0.706178    11.00000    0.04984    0.02992 =
         0.02281   -0.00397   -0.00043    0.00311
C4    1    0.704509    0.182838    0.674169    11.00000    0.04059    0.02078 =
         0.02568    0.00287    0.00253   -0.00257
C3    1    0.892498    0.301962    0.579769    11.00000    0.04331    0.03215 =
         0.02547   -0.00029    0.00866    0.00185
C6    1    1.041714    0.153240    0.539011    11.00000    0.04396    0.03927 =
         0.03506   -0.00572    0.01235    0.01244
AFIX  23
H6A   2    1.113310    0.104009    0.578766    11.00000   -1.20000
H6B   2    1.205655    0.185286    0.516143    11.00000   -1.20000
AFIX   0
C7    1    0.869221    0.118187    0.451663    11.00000    0.07870    0.05587 =
         0.04073   -0.01768    0.01141    0.01609
AFIX 137
H7A   2    0.991799    0.085307    0.410315    11.00000   -1.50000
H7B   2    0.784677    0.166556    0.414924    11.00000   -1.50000
H7C   2    0.720666    0.080240    0.473785    11.00000   -1.50000
AFIX   0
C5    1    0.738922    0.452651    0.611714    11.00000    0.08889    0.02803 =
         0.06138    0.00701    0.02579   -0.00113
AFIX 137
H5A   2    0.558368    0.480125    0.623292    11.00000   -1.50000
H5B   2    0.783399    0.460825    0.544023    11.00000   -1.50000
H5C   2    0.886396    0.479030    0.653745    11.00000   -1.50000
AFIX   0
HKLF 4




REM  cb_61_b_a.res in P2(1)/c
REM wR2 = 0.1076, GooF = S = 1.004, Restrained GooF = 1.004 for all data
REM R1 = 0.0470 for 1241 Fo > 4sig(Fo) and 0.0787 for all 1759 data
REM 120 parameters refined using 0 restraints

END

WGHT      0.0465      0.0000

REM Highest difference peak  0.567,  deepest hole -0.650,  1-sigma level  0.125
Q1    1   1.0697  0.5665  0.6808  11.00000  0.05    0.57
Q2    1   0.7334  0.0683  0.8355  11.00000  0.05    0.48
Q3    1   0.9228  0.1703  0.3200  11.00000  0.05    0.44
Q4    1   0.1263  0.2125  0.7252  11.00000  0.05    0.41
Q5    1   0.3426  0.1916  0.6829  11.00000  0.05    0.40
;
_shelx_res_checksum              37685
# end Validation Reply Form
_olex2_date_sample_data_collection 1979-12-31
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.892
_oxdiff_exptl_absorpt_empirical_full_min 0.530
# start Validation Reply Form
_vrf_PLAT431_cb_61_b             
;
PROBLEM: Short Inter HL..A Contact Br1 ..O2 . 2.97 Ang.
RESPONSE: The types of atoms were checked and the error
is indicative of short-distance intermolecular contact.
;
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Methanol-Water'
####################################################################### 
# 
# 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_20jula_chabs2
_database_code_depnum_ccdc_archive 'CCDC 2380150'
loop_
_audit_author_name
_audit_author_address
'Dr. Subrata Das'
;Associate Professor, Dept of Chemistry, NIT Patna
India
;
_audit_update_record             
;
2024-10-03 deposited with the CCDC.	2024-10-23 downloaded from the CCDC.
;
_audit_creation_date             2024-10-02
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C5 H4 Br Cl N2 O2'
_chemical_formula_sum            'C5 H4 Br Cl N2 O2'
_chemical_formula_weight         239.46
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C5 H4 Br1 N2 O2 Cl1'
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'
Br Br -0.2901 2.4595 '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'
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.9173(7)
_cell_length_b                   8.5748(4)
_cell_length_c                   8.1733(5)
_cell_angle_alpha                90
_cell_angle_beta                 109.345(7)
_cell_angle_gamma                90
_cell_volume                     721.93(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5721
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      34.4860
_cell_measurement_theta_min      3.0630
_shelx_estimated_absorpt_T_max   0.761
_shelx_estimated_absorpt_T_min   0.450
_exptl_absorpt_coefficient_mu    6.007
_exptl_absorpt_correction_T_max  0.869
_exptl_absorpt_correction_T_min  0.542
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.203
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             464.000
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 1 -1 0.0524
3 0 -8 0.0145
3 -3 1 0.0209
-3 -3 1 0.0523
-2 -1 -1 0.0629
-1 -1 0 0.0559
0 1 0 0.0504
-2 2 1 0.0115

_exptl_crystal_size_max          0.158
_exptl_crystal_size_mid          0.078
_exptl_crystal_size_min          0.048
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
1.0007 0.9996 -0.9975 0.0000 0.0940 -0.0835
3.0040 0.0019 -7.9962 -0.5040 0.2788 -0.3886
2.9962 -2.9976 0.9952 0.0632 -0.3206 -0.1351
-3.0007 -2.9985 0.9931 -0.1531 -0.1967 0.1945
-1.9988 -0.9994 -1.0022 -0.1891 0.0119 0.0825
-1.0000 -0.9994 -0.0022 -0.0765 -0.0514 0.0555
0.0005 0.9993 0.0018 0.0405 0.0720 -0.0006
-1.9987 1.9981 1.0026 0.0854 0.1428 0.1367

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0996
_diffrn_reflns_av_unetI/netI     0.0473
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            7469
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.339
_diffrn_reflns_theta_min         3.091
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.9993
_diffrn_measured_fraction_theta_max 0.9993
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -60.37 142.63   0.50    1.00    --  -22.87  73.78-130.75  406
  2  ω    -60.37 142.63   0.50    1.00    --  -22.87  73.78 127.25  406
  3  ω    -60.37 142.63   0.50    1.00    --  -22.87  73.78  25.25  406
;
_diffrn_measurement_device       'Bruker diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0360289000
_diffrn_orient_matrix_UB_12      0.0403467000
_diffrn_orient_matrix_UB_13      0.0765715000
_diffrn_orient_matrix_UB_21      -0.0206587000
_diffrn_orient_matrix_UB_22      0.0721742000
_diffrn_orient_matrix_UB_23      -0.0426050000
_diffrn_orient_matrix_UB_31      -0.0549736000
_diffrn_orient_matrix_UB_32      -0.0006123000
_diffrn_orient_matrix_UB_33      0.0279460000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1261
_reflns_number_total             1319
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.911
_refine_diff_density_min         -1.903
_refine_diff_density_rms         0.224
_refine_ls_extinction_coef       0.082(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     102
_refine_ls_number_reflns         1319
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0416
_refine_ls_restrained_S_all      1.096
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0695P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1014
_refine_ls_wR_factor_ref         0.1034
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N1(H1)
2.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Br1 Br 0.38093(3) 0.89655(4) 0.31942(4) 0.0105(2) Uani 1 1 d . . . . .
Cl1 Cl 0.11508(10) 0.92166(10) 0.43097(12) 0.0118(3) Uani 1 1 d . . . . .
O1 O 0.1007(2) 0.3594(3) 0.4634(3) 0.0124(6) Uani 1 1 d . . . . .
O2 O 0.4291(2) 0.5537(3) 0.3004(3) 0.0161(6) Uani 1 1 d . . . . .
N2 N 0.2641(3) 0.4542(4) 0.3788(3) 0.0100(6) Uani 1 1 d . . . . .
N1 N 0.1147(3) 0.6194(3) 0.4346(4) 0.0092(7) Uani 1 1 d . . . . .
H1 H 0.044391 0.633551 0.458207 0.011 Uiso 1 1 calc R U . . .
C3 C 0.2861(3) 0.7305(4) 0.3598(4) 0.0085(7) Uani 1 1 d . . . . .
C5 C 0.3075(3) 0.2937(4) 0.3675(4) 0.0135(8) Uani 1 1 d . . . . .
H5A H 0.327233 0.243931 0.478478 0.020 Uiso 1 1 calc R U . . .
H5B H 0.383814 0.295347 0.333825 0.020 Uiso 1 1 calc R U . . .
H5C H 0.239954 0.236943 0.282903 0.020 Uiso 1 1 calc R U . . .
C1 C 0.1570(3) 0.4708(4) 0.4284(4) 0.0095(7) Uani 1 1 d . . . . .
C2 C 0.3337(4) 0.5766(4) 0.3432(5) 0.0100(8) Uani 1 1 d . . . . .
C4 C 0.1790(3) 0.7459(4) 0.4051(4) 0.0082(7) Uani 1 1 d . . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Br1 0.0135(3) 0.0075(3) 0.0096(3) 0.00067(10) 0.0027(2) -0.00274(11)
Cl1 0.0150(5) 0.0068(5) 0.0130(5) -0.0013(3) 0.0037(4) 0.0029(3)
O1 0.0131(13) 0.0078(12) 0.0167(13) 0.0035(11) 0.0056(10) 0.0008(10)
O2 0.0179(13) 0.0128(14) 0.0222(15) -0.0008(12) 0.0126(11) 0.0020(12)
N2 0.0119(15) 0.0083(16) 0.0095(14) -0.0016(11) 0.0032(11) -0.0004(11)
N1 0.0091(15) 0.0082(15) 0.0116(16) 0.0009(11) 0.0051(13) 0.0002(11)
C3 0.0109(15) 0.0092(18) 0.0044(16) -0.0010(12) 0.0011(12) -0.0011(13)
C5 0.0173(17) 0.0082(18) 0.0145(18) -0.0011(13) 0.0047(14) 0.0019(13)
C1 0.0110(15) 0.0080(19) 0.0059(15) -0.0007(13) -0.0020(12) 0.0020(14)
C2 0.0149(19) 0.0069(16) 0.0054(17) -0.0021(13) -0.0002(14) -0.0006(14)
C4 0.0131(16) 0.0068(17) 0.0029(15) 0.0009(12) 0.0001(12) 0.0013(13)

_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
Br1 C3 1.853(3) . ?
Cl1 C4 1.703(3) . ?
O1 C1 1.220(5) . ?
O2 C2 1.219(5) . ?
N2 C5 1.468(4) . ?
N2 C1 1.366(4) . ?
N2 C2 1.382(5) . ?
N1 H1 0.8600 . ?
N1 C1 1.362(4) . ?
N1 C4 1.356(5) . ?
C3 C2 1.441(5) . ?
C3 C4 1.345(5) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 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
C1 N2 C5 116.3(3) . . ?
C1 N2 C2 124.6(3) . . ?
C2 N2 C5 119.1(3) . . ?
C1 N1 H1 118.7 . . ?
C4 N1 H1 118.7 . . ?
C4 N1 C1 122.7(3) . . ?
C2 C3 Br1 116.5(3) . . ?
C4 C3 Br1 124.2(3) . . ?
C4 C3 C2 119.3(3) . . ?
N2 C5 H5A 109.5 . . ?
N2 C5 H5B 109.5 . . ?
N2 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O1 C1 N2 122.4(3) . . ?
O1 C1 N1 121.3(4) . . ?
N1 C1 N2 116.3(3) . . ?
O2 C2 N2 121.3(3) . . ?
O2 C2 C3 122.9(3) . . ?
N2 C2 C3 115.8(3) . . ?
N1 C4 Cl1 115.4(2) . . ?
C3 C4 Cl1 123.4(3) . . ?
C3 C4 N1 121.2(3) . . ?

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
Br1 C3 C2 O2 -1.9(5) . . . . ?
Br1 C3 C2 N2 178.1(2) . . . . ?
Br1 C3 C4 Cl1 0.3(4) . . . . ?
Br1 C3 C4 N1 -179.3(2) . . . . ?
C5 N2 C1 O1 0.7(5) . . . . ?
C5 N2 C1 N1 -178.4(3) . . . . ?
C5 N2 C2 O2 1.0(5) . . . . ?
C5 N2 C2 C3 -179.0(3) . . . . ?
C1 N2 C2 O2 179.5(3) . . . . ?
C1 N2 C2 C3 -0.5(5) . . . . ?
C1 N1 C4 Cl1 -176.5(3) . . . . ?
C1 N1 C4 C3 3.1(6) . . . . ?
C2 N2 C1 O1 -177.8(3) . . . . ?
C2 N2 C1 N1 3.1(5) . . . . ?
C2 C3 C4 Cl1 179.2(2) . . . . ?
C2 C3 C4 N1 -0.3(5) . . . . ?
C4 N1 C1 O1 176.5(3) . . . . ?
C4 N1 C1 N2 -4.4(5) . . . . ?
C4 C3 C2 O2 179.0(4) . . . . ?
C4 C3 C2 N2 -0.9(5) . . . . ?

_shelx_res_file                  
;
TITL 20jula_chabs2_a.res in P2(1)/c
    20jula_chabs2.res
    created by SHELXL-2019/3 at 13:06:07 on 02-Oct-2024
REM Old TITL 20jula_CHabs2 in P2(1)/c
REM SHELXT solution in P2(1)/c: R1 0.089, Rweak 0.014, Alpha 0.033
REM <I/s> 1.046 for 109 systematic absences, Orientation as input
REM Formula found by SHELXT: C6 N O2 Cl Br
CELL 0.71073 10.9173 8.5748 8.1733 90 109.345 90
ZERR 4 0.0007 0.0004 0.0005 0 0.007 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H Br Cl N O
UNIT 20 16 4 4 8 8

L.S. 99
PLAN  5
SIZE 0.048 0.078 0.158
CONF
BOND
list 4
MORE -1
BOND $H
fmap 2
acta 50
SHEL 10 0.83
OMIT 1 0 0
OMIT 2 0 4
REM <olex2.extras>
REM <HklSrc "%.\\20jula_CHabs3.hkl">
REM </olex2.extras>

WGHT    0.069500
EXTI    0.082284
FVAR       4.54695
BR1   3    0.380931    0.896552    0.319418    11.00000    0.01353    0.00748 =
         0.00956    0.00067    0.00274   -0.00274
CL1   4    0.115080    0.921661    0.430966    11.00000    0.01496    0.00684 =
         0.01300   -0.00128    0.00370    0.00293
O1    6    0.100675    0.359403    0.463435    11.00000    0.01314    0.00780 =
         0.01675    0.00350    0.00560    0.00077
O2    6    0.429072    0.553665    0.300439    11.00000    0.01786    0.01276 =
         0.02221   -0.00075    0.01265    0.00202
N2    5    0.264094    0.454166    0.378813    11.00000    0.01194    0.00833 =
         0.00947   -0.00161    0.00323   -0.00042
N1    5    0.114723    0.619362    0.434621    11.00000    0.00915    0.00817 =
         0.01164    0.00093    0.00508    0.00024
AFIX  43
H1    2    0.044391    0.633551    0.458207    11.00000   -1.20000
AFIX   0
C3    1    0.286098    0.730476    0.359797    11.00000    0.01092    0.00917 =
         0.00437   -0.00097    0.00114   -0.00106
C5    1    0.307532    0.293714    0.367528    11.00000    0.01734    0.00818 =
         0.01450   -0.00106    0.00470    0.00194
AFIX 137
H5A   2    0.327233    0.243931    0.478478    11.00000   -1.50000
H5B   2    0.383814    0.295347    0.333825    11.00000   -1.50000
H5C   2    0.239954    0.236943    0.282903    11.00000   -1.50000
AFIX   0
C1    1    0.157014    0.470793    0.428432    11.00000    0.01096    0.00802 =
         0.00589   -0.00067   -0.00199    0.00200
C2    1    0.333689    0.576573    0.343192    11.00000    0.01491    0.00690 =
         0.00539   -0.00209   -0.00021   -0.00065
C4    1    0.178981    0.745864    0.405110    11.00000    0.01305    0.00684 =
         0.00291    0.00094    0.00009    0.00131
HKLF 4




REM  20jula_chabs2_a.res in P2(1)/c
REM wR2 = 0.1034, GooF = S = 1.096, Restrained GooF = 1.096 for all data
REM R1 = 0.0416 for 1261 Fo > 4sig(Fo) and 0.0427 for all 1319 data
REM 102 parameters refined using 0 restraints

END

WGHT      0.0696      0.0000

REM Highest difference peak  0.911,  deepest hole -1.903,  1-sigma level  0.224
Q1    1   0.3801  1.0040  0.3221  11.00000  0.05    0.91
Q2    1   0.2347  0.9765  0.2329  11.00000  0.05    0.72
Q3    1   0.3791  0.7843  0.3158  11.00000  0.05    0.68
Q4    1   0.4618  0.8975  0.2871  11.00000  0.05    0.65
Q5    1   0.2611  0.2463  0.5198  11.00000  0.05    0.65
;
_shelx_res_checksum              57240
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 15.793
_oxdiff_exptl_absorpt_empirical_full_min 0.460

# start Validation Reply Form
_vrf_PLAT431_20jula_chabs2       
;
PROBLEM: Short Inter HL..A Contact  Br1..O2       .     2.90 Ang.  
RESPONSE: The types of atoms were checked and the error
is indicative of short-distance intermolecular contact.
;
# end Validation Reply Form
