# Electronic Supplementary Material (ESI) for Chemical Science.
# 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. 
# 
#######################################################################

data_Q1_a
_database_code_depnum_ccdc_archive 'CCDC 2253455'
loop_
_audit_author_name
_audit_author_address
'Nahid Hassan'
;Indian Institute of Science Education and Research (IISER), Pune
India
;
_audit_update_record             
;
2023-04-02 deposited with the CCDC.	2024-02-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C4 H12 Br3 Cu2 N'
_chemical_formula_weight         440.96

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'
Cu Cu 0.3201 1.2651 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

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

_cell_length_a                   16.359(3)
_cell_length_b                   6.5479(11)
_cell_length_c                   9.5918(17)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1027.5(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9786
_cell_measurement_theta_min      2.46
_cell_measurement_theta_max      28.34

_exptl_crystal_description       niddle
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.851
_exptl_crystal_F_000             824
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    15.741
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19735
_diffrn_reflns_av_unetI/netI     0.0275
_diffrn_reflns_av_R_equivalents  0.0692
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.490
_diffrn_reflns_theta_max         28.341
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             1392
_reflns_number_gt                1325
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_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] 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-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.0149(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1392
_refine_ls_number_parameters     59
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0258
_refine_ls_R_factor_gt           0.0241
_refine_ls_wR_factor_ref         0.0971
_refine_ls_wR_factor_gt          0.0944
_refine_ls_goodness_of_fit_ref   0.860
_refine_ls_restrained_S_all      0.860
_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
Br1 Br 0.45759(2) 0.750000 0.63059(3) 0.00889(17) Uani 1 2 d S T P . .
Cu1 Cu 0.42516(2) 0.49878(5) 0.43192(4) 0.01655(18) Uani 1 1 d . . . . .
N1 N 0.6468(2) 0.750000 1.0272(3) 0.0106(6) Uani 1 2 d S T P . .
C2 C 0.6545(2) 0.9352(5) 1.1172(3) 0.0205(6) Uani 1 1 d . . . . .
H00D H 0.706501 0.933575 1.163641 0.031 Uiso 1 1 calc R U . . .
H00E H 0.611527 0.935530 1.185349 0.031 Uiso 1 1 calc R U . . .
H00F H 0.650457 1.055604 1.060511 0.031 Uiso 1 1 calc R U . . .
Br2 Br 0.39680(3) 0.750000 0.24955(4) 0.01346(18) Uani 1 2 d S T P . .
Br3 Br 0.32552(2) 0.250000 0.50566(4) 0.01302(18) Uani 1 2 d S T P . .
C3 C 0.5657(2) 0.750000 0.9569(4) 0.0166(8) Uani 1 2 d S T P . .
H00A H 0.555200 0.882763 0.918399 0.025 Uiso 0.5 1 calc R U P . .
H00B H 0.523902 0.716943 1.023514 0.025 Uiso 0.5 1 calc R U P . .
H00C H 0.565576 0.650294 0.883550 0.025 Uiso 0.5 1 calc R U P . .
C4 C 0.7123(3) 0.750000 0.9189(4) 0.0192(9) Uani 1 2 d S T P . .
H00G H 0.701857 0.856566 0.852554 0.029 Uiso 0.5 1 calc R U P . .
H00H H 0.712935 0.620475 0.872045 0.029 Uiso 0.5 1 calc R U P . .
H00I H 0.764356 0.772959 0.962516 0.029 Uiso 0.5 1 calc R U P . .

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 0.0111(2) 0.0091(3) 0.0064(2) 0.000 0.00089(12) 0.000
Cu1 0.0198(3) 0.0143(3) 0.0156(3) 0.00289(12) 0.00032(14) -0.00163(12)
N1 0.0165(16) 0.0089(14) 0.0064(15) 0.000 0.0024(12) 0.000
C2 0.0336(16) 0.0147(15) 0.0131(14) -0.0074(11) 0.0019(12) -0.0020(12)
Br2 0.0225(3) 0.0102(2) 0.0077(2) 0.000 -0.00271(13) 0.000
Br3 0.0114(3) 0.0110(3) 0.0166(3) 0.000 0.00194(13) 0.000
C3 0.016(2) 0.019(2) 0.0152(18) 0.000 -0.0010(16) 0.000
C4 0.0135(19) 0.028(2) 0.016(2) 0.000 0.0043(15) 0.000

_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 Cu1 2.5727(5) 7_575 ?
Br1 Cu1 2.5727(5) . ?
Br1 Cu1 2.5870(5) 3_656 ?
Br1 Cu1 2.5870(5) 5_666 ?
Cu1 Br3 2.4105(5) . ?
Cu1 Br2 2.4456(5) . ?
Cu1 Cu1 2.7753(8) 5_666 ?
N1 C3 1.489(5) . ?
N1 C4 1.492(5) . ?
N1 C2 1.494(3) 7_575 ?
N1 C2 1.494(3) . ?
C2 H00D 0.9600 . ?
C2 H00E 0.9600 . ?
C2 H00F 0.9600 . ?
C3 H00A 0.9600 . ?
C3 H00B 0.9600 . ?
C3 H00C 0.9600 . ?
C3 H00A 0.96(2) 7_575 ?
C3 H00B 0.960(19) 7_575 ?
C3 H00C 0.96(4) 7_575 ?
C4 H00G 0.9600 . ?
C4 H00H 0.9600 . ?
C4 H00I 0.9600 . ?
C4 H00G 0.96(6) 7_575 ?
C4 H00H 0.96(4) 7_575 ?
C4 H00I 0.96(2) 7_575 ?

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
Cu1 Br1 Cu1 79.49(2) 7_575 . ?
Cu1 Br1 Cu1 65.080(16) 7_575 3_656 ?
Cu1 Br1 Cu1 112.574(16) . 3_656 ?
Cu1 Br1 Cu1 112.575(16) 7_575 5_666 ?
Cu1 Br1 Cu1 65.080(16) . 5_666 ?
Cu1 Br1 Cu1 78.05(2) 3_656 5_666 ?
Br3 Cu1 Br2 122.42(2) . . ?
Br3 Cu1 Br1 110.747(19) . . ?
Br2 Cu1 Br1 97.981(19) . . ?
Br3 Cu1 Br1 98.269(19) . 5_666 ?
Br2 Cu1 Br1 113.477(18) . 5_666 ?
Br1 Cu1 Br1 114.920(16) . 5_666 ?
Br3 Cu1 Cu1 117.55(2) . 5_666 ?
Br2 Cu1 Cu1 120.00(2) . 5_666 ?
Br1 Cu1 Cu1 57.709(14) . 5_666 ?
Br1 Cu1 Cu1 57.212(17) 5_666 5_666 ?
C3 N1 C4 109.0(3) . . ?
C3 N1 C2 109.7(2) . 7_575 ?
C4 N1 C2 110.0(2) . 7_575 ?
C3 N1 C2 109.7(2) . . ?
C4 N1 C2 110.0(2) . . ?
C2 N1 C2 108.6(3) 7_575 . ?
N1 C2 H00D 109.5 . . ?
N1 C2 H00E 109.5 . . ?
H00D C2 H00E 109.5 . . ?
N1 C2 H00F 109.5 . . ?
H00D C2 H00F 109.5 . . ?
H00E C2 H00F 109.5 . . ?
Cu1 Br2 Cu1 84.54(2) . 7_575 ?
Cu1 Br3 Cu1 85.03(2) 7_565 . ?
N1 C3 H00A 109.5 . . ?
N1 C3 H00B 109.5 . . ?
H00A C3 H00B 109.5 . . ?
N1 C3 H00C 109.5 . . ?
H00A C3 H00C 109.5 . . ?
H00B C3 H00C 109.5 . . ?
N1 C3 H00A 109.5(5) . 7_575 ?
H00A C3 H00A 129.8 . 7_575 ?
H00B C3 H00A 85.7 . 7_575 ?
H00C C3 H00A 26.1 . 7_575 ?
N1 C3 H00B 109.5(5) . 7_575 ?
H00A C3 H00B 85.7 . 7_575 ?
H00B C3 H00B 26.1 . 7_575 ?
H00C C3 H00B 129.8 . 7_575 ?
H00A C3 H00B 109.5 7_575 7_575 ?
N1 C3 H00C 109.5(9) . 7_575 ?
H00A C3 H00C 26.1 . 7_575 ?
H00B C3 H00C 129.8 . 7_575 ?
H00C C3 H00C 85.7 . 7_575 ?
H00A C3 H00C 109.5 7_575 7_575 ?
H00B C3 H00C 109.5 7_575 7_575 ?
N1 C4 H00G 109.5 . . ?
N1 C4 H00H 109.5 . . ?
H00G C4 H00H 109.5 . . ?
N1 C4 H00I 109.5 . . ?
H00G C4 H00I 109.5 . . ?
H00H C4 H00I 109.5 . . ?
N1 C4 H00G 109.5(13) . 7_575 ?
H00G C4 H00G 93.2 . 7_575 ?
H00H C4 H00G 18.0 . 7_575 ?
H00I C4 H00G 124.1 . 7_575 ?
N1 C4 H00H 109.5(9) . 7_575 ?
H00G C4 H00H 18.0 . 7_575 ?
H00H C4 H00H 124.1 . 7_575 ?
H00I C4 H00H 93.2 . 7_575 ?
H00G C4 H00H 109.5 7_575 7_575 ?
N1 C4 H00I 109.5(5) . 7_575 ?
H00G C4 H00I 124.1 . 7_575 ?
H00H C4 H00I 93.2 . 7_575 ?
H00I C4 H00I 18.0 . 7_575 ?
H00G C4 H00I 109.5 7_575 7_575 ?
H00H C4 H00I 109.5 7_575 7_575 ?

_refine_diff_density_max         0.897
_refine_diff_density_min         -0.873
_refine_diff_density_rms         0.182

_shelx_res_file                  
;
CELL  0.71073  16.3595   6.5479   9.5918   90.000   90.000   90.000
ZERR   4   0.0030   0.0011   0.0017    0.000    0.000    0.000
LATT  1
SYMM 1/2-X, -Y, 1/2+Z
SYMM -X, 1/2+Y, -Z
SYMM 1/2+X, 1/2-Y, 1/2-Z
SFAC C H BR CU N
UNIT 16 48 12 8 4
OMIT h k l 1 0 1
OMIT h k l 0 4 0
ACTA
TEMP 23.000
L.S. 10
BOND $H
LIST 6
FMAP 2
DAMP 0.7
PLAN 20
WGHT    0.100000
EXTI    0.014936
FVAR       0.36466
BR1   3    0.457593    0.750000    0.630588    10.50000    0.01110    0.00914 =
         0.00642    0.00000    0.00089    0.00000
CU1   4    0.425155    0.498783    0.431922    11.00000    0.01984    0.01425 =
         0.01556    0.00289    0.00032   -0.00163
N1    5    0.646834    0.750000    1.027229    10.50000    0.01647    0.00891 =
         0.00638    0.00000    0.00239    0.00000
C2    1    0.654516    0.935228    1.117224    11.00000    0.03355    0.01475 =
         0.01312   -0.00741    0.00191   -0.00202
AFIX 137
H00D  2    0.706501    0.933575    1.163641    11.00000   -1.50000
H00E  2    0.611527    0.935530    1.185349    11.00000   -1.50000
H00F  2    0.650457    1.055604    1.060511    11.00000   -1.50000
AFIX   0
BR2   3    0.396805    0.750000    0.249553    10.50000    0.02253    0.01017 =
         0.00768    0.00000   -0.00271    0.00000
BR3   3    0.325521    0.250000    0.505657    10.50000    0.01140    0.01102 =
         0.01664    0.00000    0.00194    0.00000
C3    1    0.565667    0.750000    0.956927    10.50000    0.01603    0.01851 =
         0.01516    0.00000   -0.00101    0.00000
AFIX 137
H00A  2    0.555200    0.882763    0.918399    10.50000   -1.50000
H00B  2    0.523902    0.716943    1.023514    10.50000   -1.50000
H00C  2    0.565576    0.650294    0.883550    10.50000   -1.50000
AFIX   0
C4    1    0.712338    0.750000    0.918926    10.50000    0.01348    0.02844 =
         0.01568    0.00000    0.00435    0.00000
AFIX 137
H00G  2    0.701857    0.856566    0.852554    10.50000   -1.50000
H00H  2    0.712935    0.620475    0.872045    10.50000   -1.50000
H00I  2    0.764356    0.772959    0.962516    10.50000   -1.50000
REM #####
AFIX   0
HKLF 4




REM
REM wR2 = 0.097106, GooF = S = 0.86012, Restrained GooF = 0.86012 for all data
REM R1 = 0.024137 for 1325 Fo > 4sig(Fo) and 0.025759 for all 1392 data
REM 59 parameters refined using 0 restraints

END

WGHT      0.0338      1.5087

REM Highest difference peak  0.897,  deepest hole -0.873,  1-sigma level  0.182
Q1    1   0.3501  0.7500  0.1987  10.50000  0.05    0.90
Q2    1   0.3466  0.7500  0.3184  10.50000  0.05    0.71
Q3    1   0.6688  0.7500  0.9936  10.50000  0.05    0.68
Q4    1   0.5701  0.9916  0.9392  11.00000  0.05    0.62
Q5    1   0.3691  0.8684  0.2572  11.00000  0.05    0.61
Q6    1   0.4819  0.8652  0.6282  11.00000  0.05    0.58
Q7    1   0.4029  0.3778  0.4190  11.00000  0.05    0.57
Q8    1   0.4635  1.0015  0.6871  11.00000  0.05    0.54
Q9    1   0.3596  0.1202  0.5115  11.00000  0.05    0.54
Q10   1   0.4629  0.7500  0.8648  10.50000  0.05    0.53
Q11   1   0.7681  0.4895  0.9300  11.00000  0.05    0.52
Q12   1   0.4350  0.4963  0.5816  11.00000  0.05    0.52
Q13   1   0.3011  0.1203  0.5132  11.00000  0.05    0.51
Q14   1   0.6704  1.0057  0.8257  11.00000  0.05    0.51
Q15   1   0.6409  0.8397  1.0543  11.00000  0.05    0.50
Q16   1   0.6090  0.7500  0.9971  10.50000  0.05    0.49
Q17   1   0.5136  1.0039  1.1907  11.00000  0.05    0.49
Q18   1   0.5053  0.7500  0.6906  10.50000  0.05    0.47
Q19   1   0.4190  0.3748  0.5228  11.00000  0.05    0.47
Q20   1   0.6973  1.0366  1.1748  11.00000  0.05    0.46
;
_shelx_res_checksum              71293
####################################################################### 
# 
# 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_TRY_a
_database_code_depnum_ccdc_archive 'CCDC 2309331'
loop_
_audit_author_name
_audit_author_address
'Nahid Hassan'
;Indian Institute of Science Education and Research (IISER), Pune
India
;
_audit_update_record             
;
2023-11-21 deposited with the CCDC.	2024-02-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/1
_shelx_SHELXL_version_number     2019/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Ag2 Br3, C4 H12 N'
_chemical_formula_sum            'C4 H12 Ag2 Br3 N'
_chemical_formula_weight         529.62

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'
Ag Ag -0.8971 1.1015 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

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

_cell_length_a                   16.535(2)
_cell_length_b                   7.0771(9)
_cell_length_c                   9.6517(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1129.4(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9983
_cell_measurement_theta_min      2.46
_cell_measurement_theta_max      25.03

_exptl_crystal_description       Needle
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.115
_exptl_crystal_F_000             968
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          1.000
_exptl_crystal_size_mid          0.076
_exptl_crystal_size_min          0.074
_exptl_absorpt_coefficient_mu    14.022
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2833
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15396
_diffrn_reflns_av_unetI/netI     0.0179
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.443
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_full        25.027
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             1087
_reflns_number_gt                1009
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0262P)²+0.3033P] 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     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1087
_refine_ls_number_parameters     58
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0252
_refine_ls_R_factor_gt           0.0222
_refine_ls_wR_factor_ref         0.0489
_refine_ls_wR_factor_gt          0.0480
_refine_ls_goodness_of_fit_ref   1.217
_refine_ls_restrained_S_all      1.217
_refine_ls_shift/su_max          0.001
_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
Ag1 Ag 0.42040(2) 0.49756(3) 0.57957(3) 0.02577(12) Uani 1 1 d . . . . .
Br1 Br 0.45040(3) 0.750000 0.36287(4) 0.01611(13) Uani 1 2 d S T P . .
Br2 Br 0.39770(3) 0.750000 0.77831(5) 0.02556(14) Uani 1 2 d S T P . .
Br3 Br 0.31064(3) 0.250000 0.50893(6) 0.02694(15) Uani 1 2 d S T P . .
N1 N 0.3549(2) 0.250000 0.0374(4) 0.0172(8) Uani 1 2 d S T P . .
C11 C 0.3552(3) 0.4219(4) 0.1275(4) 0.0340(9) Uani 1 1 d . . . . .
H11A H 0.306357 0.422982 0.185019 0.051 Uiso 1 1 calc R U . . .
H11B H 0.356311 0.535329 0.069337 0.051 Uiso 1 1 calc R U . . .
H11C H 0.403123 0.419873 0.187209 0.051 Uiso 1 1 calc R U . . .
C12 C 0.2820(3) 0.250000 -0.0531(6) 0.0350(13) Uani 1 2 d S T P . .
H12A H 0.233370 0.236198 0.004215 0.052 Uiso 0.5 1 calc R U P A -1
H12B H 0.285235 0.144470 -0.118558 0.052 Uiso 0.5 1 calc R U P A -1
H12C H 0.279237 0.369331 -0.104358 0.052 Uiso 0.5 1 calc R U P A -1
C13 C 0.4285(3) 0.250000 -0.0506(5) 0.0296(12) Uani 1 2 d S T P . .
H13A H 0.429735 0.365314 -0.106817 0.044 Uiso 0.5 1 calc R U P B -1
H13B H 0.427766 0.139329 -0.111653 0.044 Uiso 0.5 1 calc R U P B -1
H13C H 0.476672 0.245358 0.008464 0.044 Uiso 0.5 1 calc R U P B -1

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
Ag1 0.02926(19) 0.01945(18) 0.0286(2) -0.00078(10) 0.00044(12) -0.00069(9)
Br1 0.0189(3) 0.0131(2) 0.0164(2) 0.000 -0.00122(18) 0.000
Br2 0.0388(3) 0.0177(2) 0.0202(3) 0.000 0.0043(2) 0.000
Br3 0.0206(3) 0.0177(2) 0.0425(3) 0.000 -0.0039(2) 0.000
N1 0.019(2) 0.0161(18) 0.0168(18) 0.000 -0.0044(16) 0.000
C11 0.055(3) 0.0179(18) 0.0288(19) -0.0094(16) 0.0009(18) 0.0054(17)
C12 0.027(3) 0.036(3) 0.043(3) 0.000 -0.016(3) 0.000
C13 0.027(3) 0.027(3) 0.034(3) 0.000 0.007(2) 0.000

_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
Ag1 Br3 2.6131(5) . ?
Ag1 Br2 2.6480(5) . ?
Ag1 Br1 2.7950(5) . ?
Ag1 Br1 2.8181(5) 5_666 ?
Ag1 Ag1 3.0477(6) 5_666 ?
N1 C13 1.485(6) . ?
N1 C12 1.489(6) . ?
N1 C11 1.495(4) . ?
N1 C11 1.495(4) 7_565 ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br3 Ag1 Br2 122.879(19) . . ?
Br3 Ag1 Br1 110.890(17) . . ?
Br2 Ag1 Br1 97.814(15) . . ?
Br3 Ag1 Br1 99.272(15) . 5_666 ?
Br2 Ag1 Br1 112.587(17) . 5_666 ?
Br1 Ag1 Br1 114.229(13) . 5_666 ?
Br3 Ag1 Ag1 118.424(18) . 5_666 ?
Br2 Ag1 Ag1 118.675(17) . 5_666 ?
Br1 Ag1 Ag1 57.479(12) . 5_666 ?
Br1 Ag1 Ag1 56.750(13) 5_666 5_666 ?
Ag1 Br1 Ag1 79.464(17) 7_575 . ?
Ag1 Br1 Ag1 65.769(13) 7_575 3_656 ?
Ag1 Br1 Ag1 112.604(16) . 3_656 ?
Ag1 Br1 Ag1 112.604(16) 7_575 5_666 ?
Ag1 Br1 Ag1 65.770(13) . 5_666 ?
Ag1 Br1 Ag1 76.879(17) 3_656 5_666 ?
Ag1 Br2 Ag1 84.856(19) . 7_575 ?
Ag1 Br3 Ag1 84.20(2) . 7_565 ?
C13 N1 C12 109.2(4) . . ?
C13 N1 C11 109.3(2) . . ?
C12 N1 C11 110.1(2) . . ?
C13 N1 C11 109.3(2) . 7_565 ?
C12 N1 C11 110.1(2) . 7_565 ?
C11 N1 C11 108.8(4) . 7_565 ?
N1 C11 H11A 109.5 . . ?
N1 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N1 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N1 C12 H12A 109.5 . . ?
N1 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N1 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N1 C13 H13A 109.5 . . ?
N1 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N1 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?


_refine_diff_density_max         0.598
_refine_diff_density_min         -1.399
_refine_diff_density_rms         0.264

_shelx_res_file                  
;
TITL TRY_a.res in Pnma
    TRY_a.res
    created by SHELXL-2019/1 at 12:32:12 on 10-Oct-2023
REM Old TITL TRY in Pnma
REM SHELXT solution in Pnma: R1 0.084, Rweak 0.003, Alpha 0.009
REM <I/s> 0.891 for 114 systematic absences, Orientation as input
REM Formula found by SHELXT: C4 Ag2 Br3 N
REM LIST 6
CELL 0.71073 16.5351 7.0771 9.6517 90 90 90
ZERR 4 0.002 0.0009 0.0011 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,-Z
SYMM 0.5+X,0.5-Y,0.5-Z
SFAC C H Ag Br N
UNIT 16 48 8 12 4

L.S. 80
PLAN  4
TEMP -123
CONF
LIST 4
BOND
MORE -1
BOND $H
fmap 2
acta
OMIT 5 0 2
REM <olex2.extras>
REM <HklSrc "%.\\TRY_a.hkl">
REM </olex2.extras>

WGHT    0.026200    0.303300
FVAR       0.22582
AG1   3    0.420404    0.497558    0.579568    11.00000    0.02926    0.01945 =
         0.02861   -0.00078    0.00044   -0.00069
BR1   4    0.450399    0.750000    0.362871    10.50000    0.01892    0.01306 =
         0.01635    0.00000   -0.00122    0.00000
BR2   4    0.397701    0.750000    0.778309    10.50000    0.03881    0.01766 =
         0.02020    0.00000    0.00435    0.00000
BR3   4    0.310639    0.250000    0.508933    10.50000    0.02059    0.01768 =
         0.04254    0.00000   -0.00394    0.00000
N1    5    0.354878    0.250000    0.037363    10.50000    0.01851    0.01613 =
         0.01684    0.00000   -0.00437    0.00000
C11   1    0.355195    0.421852    0.127498    11.00000    0.05520    0.01788 =
         0.02883   -0.00944    0.00093    0.00538
AFIX 137
H11A  2    0.306357    0.422982    0.185019    11.00000   -1.50000
H11B  2    0.356311    0.535329    0.069337    11.00000   -1.50000
H11C  2    0.403123    0.419873    0.187209    11.00000   -1.50000
AFIX   0
C12   1    0.281951    0.250000   -0.053057    10.50000    0.02682    0.03557 =
         0.04257    0.00000   -0.01620    0.00000
PART -1
AFIX 137
H12A  2    0.233370    0.236198    0.004215    10.50000   -1.50000
H12B  2    0.285235    0.144470   -0.118558    10.50000   -1.50000
H12C  2    0.279237    0.369331   -0.104358    10.50000   -1.50000
AFIX   0
PART 0
C13   1    0.428521    0.250000   -0.050639    10.50000    0.02717    0.02719 =
         0.03433    0.00000    0.00742    0.00000
PART -1
AFIX 137
H13A  2    0.429735    0.365314   -0.106817    10.50000   -1.50000
H13B  2    0.427766    0.139329   -0.111653    10.50000   -1.50000
H13C  2    0.476672    0.245358    0.008464    10.50000   -1.50000
AFIX   0
HKLF 4




REM  TRY_a.res in Pnma
REM wR2 = 0.0489, GooF = S = 1.217, Restrained GooF = 1.217 for all data
REM R1 = 0.0222 for 1009 Fo > 4sig(Fo) and 0.0252 for all 1087 data
REM 58 parameters refined using 0 restraints

END

WGHT      0.0261      0.3038

REM Highest difference peak  0.598,  deepest hole -1.399,  1-sigma level  0.264
Q1    1   0.3355  0.8780  0.6637  11.00000  0.05    0.60
Q2    1   0.2406  0.1291  0.5482  11.00000  0.05    0.56
Q3    1   0.4424  0.3436  0.1831  11.00000  0.05    0.56
Q4    1   0.2866  0.3863  0.1397  11.00000  0.05    0.54
;
_shelx_res_checksum              57630
