# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_MIAu_a
_database_code_depnum_ccdc_archive 'CCDC 2176097'
loop_
_audit_author_name
_audit_author_address
'Arnab Rit'
;IIT Madras
India
;
_audit_update_record             
;
2022-05-31 deposited with the CCDC.	2022-10-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H11 Au Br N3'
_chemical_formula_weight         450.09

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'
Au Au -2.0133 8.8022 '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'

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

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.0635(2)
_cell_length_b                   9.6309(4)
_cell_length_c                   11.0320(5)
_cell_angle_alpha                101.765(2)
_cell_angle_beta                 104.967(2)
_cell_angle_gamma                97.601(2)
_cell_volume                     597.54(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5768
_cell_measurement_theta_min      2.57
_cell_measurement_theta_max      26.32

_exptl_crystal_description       Rectangular
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.502
_exptl_crystal_F_000             412
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    15.624
_shelx_estimated_absorpt_T_min   0.203
_shelx_estimated_absorpt_T_max   0.304
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.203
_exptl_absorpt_correction_T_max  0.304
_exptl_absorpt_process_details   'SADABS V2014/5(Bruker AXS.Inc)'
_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            7349
_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.973
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             2102
_reflns_number_gt                1942
_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    '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)+(0.0505P)²+4.5513P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0116(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2102
_refine_ls_number_parameters     129
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0340
_refine_ls_wR_factor_ref         0.0947
_refine_ls_wR_factor_gt          0.0922
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_restrained_S_all      1.079
_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
C7 C 0.2782(9) 0.5580(6) 0.2264(5) 0.0330(18) Uani 1 1 d G . . . .
C8 C 0.0997(11) 0.4412(6) 0.1440(4) 0.044(2) Uani 1 1 d G . . . .
H8 H 0.0919 0.3922 0.0606 0.053 Uiso 1 1 calc R U . . .
N1 N -0.0650(8) 0.4122(5) 0.2112(5) 0.0407(17) Uani 1 1 d G . . . .
N2 N 0.0118(9) 0.5112(5) 0.3351(4) 0.0370(16) Uani 1 1 d G . . . .
N3 N 0.2239(8) 0.6012(5) 0.3445(4) 0.0380(16) Uani 1 1 d G . . . .
Au1 Au 0.54499(6) 0.66749(3) 0.19027(3) 0.03670(19) Uani 1 1 d . . . . .
C1 C 0.3259(16) 0.7074(10) 0.4510(8) 0.0371(19) Uani 1 1 d . . . . .
C2 C 0.1964(19) 0.8065(11) 0.4913(9) 0.046(2) Uani 1 1 d . . . . .
H2 H 0.0392 0.7967 0.4489 0.055 Uiso 1 1 calc R U . . .
C3 C 0.314(2) 0.9220(11) 0.5986(10) 0.055(3) Uani 1 1 d . . . . .
H3 H 0.2341 0.9917 0.6278 0.066 Uiso 1 1 calc R U . . .
C4 C 0.544(2) 0.9334(13) 0.6611(10) 0.063(3) Uani 1 1 d . . . . .
H4 H 0.6190 1.0097 0.7332 0.075 Uiso 1 1 calc R U . . .
C5 C 0.668(2) 0.8323(14) 0.6182(11) 0.063(3) Uani 1 1 d . . . . .
H5 H 0.8254 0.8420 0.6611 0.076 Uiso 1 1 calc R U . . .
C6 C 0.5596(18) 0.7170(12) 0.5117(9) 0.049(2) Uani 1 1 d . . . . .
H6 H 0.6409 0.6486 0.4821 0.059 Uiso 1 1 calc R U . . .
C9 C -0.2741(19) 0.3160(10) 0.1725(10) 0.050(2) Uani 1 1 d . . . . .
H9A H -0.3934 0.3556 0.1210 0.060 Uiso 1 1 calc R U . . .
H9B H -0.3188 0.3028 0.2483 0.060 Uiso 1 1 calc R U . . .
C10 C -0.260(2) 0.1753(12) 0.0961(12) 0.062(3) Uani 1 1 d . . . . .
H10A H -0.2257 0.1872 0.0181 0.093 Uiso 1 1 calc R U . . .
H10B H -0.4056 0.1095 0.0743 0.093 Uiso 1 1 calc R U . . .
H10C H -0.1384 0.1373 0.1459 0.093 Uiso 1 1 calc R U . . .
Br1 Br 0.8587(2) 0.80146(12) 0.14407(11) 0.0569(3) Uani 1 1 d . . . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C7 N3 1.4200 . ?
C7 C8 1.4200 . ?
C7 Au1 1.985(4) . ?
C8 N1 1.4200 . ?
C8 H8 0.9300 . ?
N1 C9 1.377(10) . ?
N1 N2 1.4200 . ?
N2 N3 1.4200 . ?
N3 C1 1.333(9) . ?
Au1 Br1 2.3795(12) . ?
C1 C6 1.384(14) . ?
C1 C2 1.389(14) . ?
C2 C3 1.402(14) . ?
C2 H2 0.9300 . ?
C3 C4 1.369(17) . ?
C3 H3 0.9300 . ?
C4 C5 1.387(18) . ?
C4 H4 0.9300 . ?
C5 C6 1.387(15) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C9 C10 1.469(15) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 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
N3 C7 C8 108.0 . . ?
N3 C7 Au1 121.7(3) . . ?
C8 C7 Au1 130.0(3) . . ?
C7 C8 N1 108.0 . . ?
C7 C8 H8 126.0 . . ?
N1 C8 H8 126.0 . . ?
C9 N1 C8 131.2(6) . . ?
C9 N1 N2 120.7(6) . . ?
C8 N1 N2 108.0 . . ?
N3 N2 N1 108.0 . . ?
C1 N3 C7 132.7(5) . . ?
C1 N3 N2 119.2(5) . . ?
C7 N3 N2 108.0 . . ?
C7 Au1 Br1 178.67(19) . . ?
N3 C1 C6 117.8(8) . . ?
N3 C1 C2 118.6(8) . . ?
C6 C1 C2 123.5(9) . . ?
C1 C2 C3 116.9(10) . . ?
C1 C2 H2 121.5 . . ?
C3 C2 H2 121.5 . . ?
C4 C3 C2 120.7(11) . . ?
C4 C3 H3 119.7 . . ?
C2 C3 H3 119.7 . . ?
C3 C4 C5 120.8(10) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 H4 119.6 . . ?
C6 C5 C4 120.4(11) . . ?
C6 C5 H5 119.8 . . ?
C4 C5 H5 119.8 . . ?
C1 C6 C5 117.6(10) . . ?
C1 C6 H6 121.2 . . ?
C5 C6 H6 121.2 . . ?
N1 C9 C10 111.6(9) . . ?
N1 C9 H9A 109.3 . . ?
C10 C9 H9A 109.3 . . ?
N1 C9 H9B 109.3 . . ?
C10 C9 H9B 109.3 . . ?
H9A C9 H9B 108.0 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 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
N3 C7 C8 N1 0.0 . . . . ?
Au1 C7 C8 N1 -173.2(5) . . . . ?
C7 C8 N1 C9 176.1(9) . . . . ?
C7 C8 N1 N2 0.0 . . . . ?
C9 N1 N2 N3 -176.6(8) . . . . ?
C8 N1 N2 N3 0.0 . . . . ?
C8 C7 N3 C1 -176.9(8) . . . . ?
Au1 C7 N3 C1 -3.0(9) . . . . ?
C8 C7 N3 N2 0.0 . . . . ?
Au1 C7 N3 N2 173.9(5) . . . . ?
N1 N2 N3 C1 177.4(7) . . . . ?
N1 N2 N3 C7 0.0 . . . . ?
C7 N3 C1 C6 -53.8(11) . . . . ?
N2 N3 C1 C6 129.6(7) . . . . ?
C7 N3 C1 C2 122.8(8) . . . . ?
N2 N3 C1 C2 -53.8(10) . . . . ?
N3 C1 C2 C3 -175.9(8) . . . . ?
C6 C1 C2 C3 0.5(14) . . . . ?
C1 C2 C3 C4 -1.1(15) . . . . ?
C2 C3 C4 C5 1.2(17) . . . . ?
C3 C4 C5 C6 -0.6(18) . . . . ?
N3 C1 C6 C5 176.4(9) . . . . ?
C2 C1 C6 C5 0.0(15) . . . . ?
C4 C5 C6 C1 0.1(16) . . . . ?
C8 N1 C9 C10 41.6(12) . . . . ?
N2 N1 C9 C10 -142.7(8) . . . . ?

_refine_diff_density_max         1.980
_refine_diff_density_min         -1.846
_refine_diff_density_rms         0.190



####################################################################### 
# 
# 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_mi3
_database_code_depnum_ccdc_archive 'CCDC 2176103'
loop_
_audit_author_name
_audit_author_address
'Arnab Rit'
;IIT Madras
India
;
_audit_update_record             
;
2022-05-31 deposited with the CCDC.	2022-10-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C25 H31 Au Br Cl Ir N5'
_chemical_formula_sum            'C25 H31 Au Br Cl Ir N5'
_chemical_formula_weight         906.07

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Au Au -2.0133 8.8022 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   9.6523(9)
_cell_length_b                   25.471(3)
_cell_length_c                   11.1422(12)
_cell_angle_alpha                90
_cell_angle_beta                 104.835(5)
_cell_angle_gamma                90
_cell_volume                     2648.0(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1428
_cell_measurement_theta_min      2.48
_cell_measurement_theta_max      21.94

_exptl_crystal_description       Block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.273
_exptl_crystal_F_000             1696
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    12.188
_shelx_estimated_absorpt_T_min   0.375
_shelx_estimated_absorpt_T_max   0.581
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.375
_exptl_absorpt_correction_T_max  0.581
_exptl_absorpt_process_details   'SADABS V2014/5(Bruker AXS.Inc)'
_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            13474
_diffrn_reflns_av_unetI/netI     0.0730
_diffrn_reflns_av_R_equivalents  0.0847
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.053
_diffrn_reflns_theta_max         22.151
_diffrn_reflns_theta_full        22.151
_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             3309
_reflns_number_gt                2501
_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    '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)+(0.0543P)²+64.0144P] 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         3309
_refine_ls_number_parameters     314
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0743
_refine_ls_R_factor_gt           0.0492
_refine_ls_wR_factor_ref         0.1317
_refine_ls_wR_factor_gt          0.1179
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.027
_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
Au1 Au 0.97897(8) -0.10370(3) 0.51924(6) 0.0309(3) Uani 1 1 d . . . . .
Br1 Br 0.2802(3) 0.05447(11) -0.0721(2) 0.0661(8) Uani 1 1 d . . . . .
C1 C 0.5858(17) 0.1175(7) -0.1065(15) 0.022(4) Uani 1 1 d . U . . .
C2 C 0.4877(18) 0.1593(8) -0.1642(16) 0.031(5) Uani 1 1 d . . . . .
C3 C 0.5083(18) 0.2019(7) -0.0715(16) 0.026(5) Uani 1 1 d . . . . .
C4 C 0.6149(17) 0.1834(8) 0.0391(14) 0.023(4) Uani 1 1 d . . . . .
C5 C 0.6674(17) 0.1336(7) 0.0101(16) 0.024(4) Uani 1 1 d . . . . .
C6 C 0.7922(18) 0.1037(9) 0.0923(17) 0.037(5) Uani 1 1 d . . . . .
H6A H 0.8794 0.1136 0.0720 0.055 Uiso 1 1 calc R U . . .
H6B H 0.7769 0.0667 0.0792 0.055 Uiso 1 1 calc R U . . .
H6C H 0.7992 0.1119 0.1778 0.055 Uiso 1 1 calc R U . . .
C7 C 0.603(2) 0.0677(7) -0.1744(16) 0.031(5) Uani 1 1 d . . . . .
H7A H 0.6666 0.0740 -0.2264 0.046 Uiso 1 1 calc R U . . .
H7B H 0.5112 0.0568 -0.2246 0.046 Uiso 1 1 calc R U . . .
H7C H 0.6420 0.0407 -0.1153 0.046 Uiso 1 1 calc R U . . .
C8 C 0.394(2) 0.1598(8) -0.2905(15) 0.032(5) Uani 1 1 d . . . . .
H8A H 0.4519 0.1586 -0.3491 0.049 Uiso 1 1 calc R U . . .
H8B H 0.3382 0.1914 -0.3030 0.049 Uiso 1 1 calc R U . . .
H8C H 0.3319 0.1299 -0.3021 0.049 Uiso 1 1 calc R U . . .
C9 C 0.442(2) 0.2535(7) -0.0864(16) 0.033(5) Uani 1 1 d . . . . .
H9A H 0.4170 0.2632 -0.0112 0.049 Uiso 1 1 calc R U . . .
H9B H 0.3566 0.2527 -0.1537 0.049 Uiso 1 1 calc R U . . .
H9C H 0.5075 0.2788 -0.1041 0.049 Uiso 1 1 calc R U . . .
C10 C 0.680(2) 0.2183(8) 0.1491(17) 0.039(5) Uani 1 1 d . . . . .
H10A H 0.7080 0.1973 0.2229 0.059 Uiso 1 1 calc R U . . .
H10B H 0.6108 0.2439 0.1587 0.059 Uiso 1 1 calc R U . . .
H10C H 0.7627 0.2358 0.1352 0.059 Uiso 1 1 calc R U . . .
C11 C 0.2718(16) 0.1611(7) 0.0665(14) 0.017(4) Uani 1 1 d . U . . .
C12 C 0.078(2) 0.2001(8) 0.1018(16) 0.034(5) Uani 1 1 d . . . . .
H12 H -0.0050 0.2202 0.0893 0.041 Uiso 1 1 calc R U . . .
C13 C 0.1489(18) 0.1772(7) 0.2098(16) 0.024(4) Uani 1 1 d . . . . .
H13 H 0.1216 0.1765 0.2840 0.029 Uiso 1 1 calc R U . . .
C14 C 0.3774(17) 0.1233(7) 0.2616(16) 0.026(5) Uani 1 1 d . . . . .
C15 C 0.388(2) 0.1121(8) 0.3840(15) 0.030(5) Uani 1 1 d . . . . .
H15 H 0.3227 0.1262 0.4242 0.037 Uiso 1 1 calc R U . . .
C16 C 0.4969(19) 0.0795(8) 0.4459(16) 0.031(5) Uani 1 1 d . . . . .
H16 H 0.5099 0.0730 0.5302 0.037 Uiso 1 1 calc R U . . .
C17 C 0.5845(17) 0.0572(7) 0.3845(15) 0.024(4) Uani 1 1 d . U . . .
C18 C 0.5714(18) 0.0676(8) 0.2553(15) 0.027(5) Uani 1 1 d . . . . .
H18 H 0.6328 0.0512 0.2149 0.033 Uiso 1 1 calc R U . . .
C19 C 0.4681(17) 0.1019(7) 0.1910(15) 0.022(4) Uani 1 1 d . . . . .
C20 C 0.8591(19) -0.0395(8) 0.5040(16) 0.029(5) Uani 1 1 d . . . . .
C21 C 0.7573(16) -0.0191(7) 0.4068(15) 0.022(4) Uani 1 1 d . . . . .
H21 H 0.7325 -0.0324 0.3263 0.026 Uiso 1 1 calc R U . . .
C22 C 0.951(2) -0.0029(11) 0.7301(19) 0.060(8) Uani 1 1 d . . . . .
H22A H 1.0437 -0.0179 0.7317 0.072 Uiso 1 1 calc R U . . .
H22B H 0.9653 0.0335 0.7558 0.072 Uiso 1 1 calc R U . . .
C23 C 0.891(2) -0.0298(11) 0.811(2) 0.060(7) Uani 1 1 d . . . . .
H23A H 0.8054 -0.0120 0.8183 0.090 Uiso 1 1 calc R U . . .
H23B H 0.9578 -0.0314 0.8913 0.090 Uiso 1 1 calc R U . . .
H23C H 0.8667 -0.0647 0.7807 0.090 Uiso 1 1 calc R U . . .
C24 C 0.0963(19) 0.1980(8) -0.1177(15) 0.033(5) Uani 1 1 d . . . . .
H24A H 0.1699 0.1898 -0.1600 0.040 Uiso 1 1 calc R U . . .
H24B H 0.0726 0.2349 -0.1311 0.040 Uiso 1 1 calc R U . . .
C25 C -0.034(2) 0.1655(9) -0.1717(16) 0.052(6) Uani 1 1 d . . . . .
H25A H -0.0089 0.1290 -0.1662 0.079 Uiso 1 1 calc R U . . .
H25B H -0.0731 0.1749 -0.2571 0.079 Uiso 1 1 calc R U . . .
H25C H -0.1049 0.1718 -0.1262 0.079 Uiso 1 1 calc R U . . .
Cl1 Cl 1.1137(5) -0.17970(19) 0.5371(4) 0.0330(12) Uani 1 1 d . . . . .
Ir1 Ir 0.43786(7) 0.13045(3) 0.01417(6) 0.0190(2) Uani 1 1 d . . . . .
N1 N 0.1511(14) 0.1884(6) 0.0136(13) 0.026(4) Uani 1 1 d . . . . .
N2 N 0.2679(13) 0.1554(6) 0.1872(12) 0.020(3) Uani 1 1 d . . . . .
N3 N 0.6989(14) 0.0232(6) 0.4467(11) 0.020(3) Uani 1 1 d . . . . .
N4 N 0.7597(17) 0.0325(7) 0.5659(13) 0.039(4) Uani 1 1 d . . . . .
N5 N 0.8547(17) -0.0056(7) 0.5991(14) 0.040(4) Uani 1 1 d . . . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Au1 C20 1.986(19) . ?
Au1 Cl1 2.312(5) . ?
Br1 Ir1 2.497(3) . ?
C1 C5 1.40(2) . ?
C1 C2 1.46(3) . ?
C1 C7 1.51(2) . ?
C1 Ir1 2.222(16) . ?
C2 C8 1.46(2) . ?
C2 C3 1.48(3) . ?
C2 Ir1 2.283(17) . ?
C3 C9 1.45(2) . ?
C3 C4 1.47(2) . ?
C3 Ir1 2.240(17) . ?
C4 C5 1.43(3) . ?
C4 C10 1.51(2) . ?
C4 Ir1 2.138(17) . ?
C5 C6 1.52(3) . ?
C5 Ir1 2.230(15) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 N1 1.36(2) . ?
C11 N2 1.36(2) . ?
C11 Ir1 1.999(15) . ?
C12 C13 1.36(3) . ?
C12 N1 1.38(2) . ?
C12 H12 0.9300 . ?
C13 N2 1.36(2) . ?
C13 H13 0.9300 . ?
C14 C15 1.37(2) . ?
C14 N2 1.42(2) . ?
C14 C19 1.43(2) . ?
C15 C16 1.38(3) . ?
C15 H15 0.9300 . ?
C16 C17 1.34(2) . ?
C16 H16 0.9300 . ?
C17 N3 1.43(2) . ?
C17 C18 1.44(2) . ?
C18 C19 1.38(3) . ?
C18 H18 0.9300 . ?
C19 Ir1 2.050(17) . ?
C20 C21 1.36(2) . ?
C20 N5 1.38(2) . ?
C21 N3 1.34(2) . ?
C21 H21 0.9300 . ?
C22 C23 1.38(3) . ?
C22 N5 1.52(3) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 N1 1.44(2) . ?
C24 C25 1.50(3) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
N3 N4 1.329(19) . ?
N4 N5 1.32(2) . ?

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
C20 Au1 Cl1 178.6(5) . . ?
C5 C1 C2 110.1(16) . . ?
C5 C1 C7 127.2(16) . . ?
C2 C1 C7 122.3(15) . . ?
C5 C1 Ir1 72.0(9) . . ?
C2 C1 Ir1 73.4(9) . . ?
C7 C1 Ir1 126.8(12) . . ?
C1 C2 C8 126.9(17) . . ?
C1 C2 C3 105.7(15) . . ?
C8 C2 C3 127.3(17) . . ?
C1 C2 Ir1 68.8(10) . . ?
C8 C2 Ir1 128.7(12) . . ?
C3 C2 Ir1 69.4(9) . . ?
C9 C3 C4 125.6(17) . . ?
C9 C3 C2 127.4(16) . . ?
C4 C3 C2 106.9(15) . . ?
C9 C3 Ir1 127.6(12) . . ?
C4 C3 Ir1 66.7(9) . . ?
C2 C3 Ir1 72.5(11) . . ?
C5 C4 C3 107.9(15) . . ?
C5 C4 C10 127.2(16) . . ?
C3 C4 C10 123.2(17) . . ?
C5 C4 Ir1 74.3(10) . . ?
C3 C4 Ir1 74.2(10) . . ?
C10 C4 Ir1 128.9(12) . . ?
C1 C5 C4 108.7(15) . . ?
C1 C5 C6 125.9(17) . . ?
C4 C5 C6 125.4(16) . . ?
C1 C5 Ir1 71.4(9) . . ?
C4 C5 Ir1 67.4(9) . . ?
C6 C5 Ir1 127.5(11) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C1 C7 H7A 109.5 . . ?
C1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C2 C8 H8A 109.5 . . ?
C2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C3 C9 H9A 109.5 . . ?
C3 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C3 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C4 C10 H10A 109.5 . . ?
C4 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C4 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C11 N2 104.2(13) . . ?
N1 C11 Ir1 137.6(12) . . ?
N2 C11 Ir1 118.3(11) . . ?
C13 C12 N1 107.7(16) . . ?
C13 C12 H12 126.1 . . ?
N1 C12 H12 126.1 . . ?
N2 C13 C12 105.7(15) . . ?
N2 C13 H13 127.2 . . ?
C12 C13 H13 127.2 . . ?
C15 C14 N2 123.5(16) . . ?
C15 C14 C19 124.9(17) . . ?
N2 C14 C19 111.6(14) . . ?
C14 C15 C16 118.2(17) . . ?
C14 C15 H15 120.9 . . ?
C16 C15 H15 120.9 . . ?
C17 C16 C15 120.1(16) . . ?
C17 C16 H16 120.0 . . ?
C15 C16 H16 120.0 . . ?
C16 C17 N3 121.1(15) . . ?
C16 C17 C18 121.8(17) . . ?
N3 C17 C18 117.1(15) . . ?
C19 C18 C17 120.2(17) . . ?
C19 C18 H18 119.9 . . ?
C17 C18 H18 119.9 . . ?
C18 C19 C14 114.8(15) . . ?
C18 C19 Ir1 129.0(12) . . ?
C14 C19 Ir1 116.0(13) . . ?
C21 C20 N5 102.5(16) . . ?
C21 C20 Au1 131.7(14) . . ?
N5 C20 Au1 125.6(14) . . ?
N3 C21 C20 108.6(15) . . ?
N3 C21 H21 125.7 . . ?
C20 C21 H21 125.7 . . ?
C23 C22 N5 110.6(18) . . ?
C23 C22 H22A 109.5 . . ?
N5 C22 H22A 109.5 . . ?
C23 C22 H22B 109.5 . . ?
N5 C22 H22B 109.5 . . ?
H22A C22 H22B 108.1 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N1 C24 C25 111.4(15) . . ?
N1 C24 H24A 109.4 . . ?
C25 C24 H24A 109.4 . . ?
N1 C24 H24B 109.4 . . ?
C25 C24 H24B 109.4 . . ?
H24A C24 H24B 108.0 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C11 Ir1 C19 77.6(7) . . ?
C11 Ir1 C4 113.0(7) . . ?
C19 Ir1 C4 100.7(6) . . ?
C11 Ir1 C1 157.2(6) . . ?
C19 Ir1 C1 125.0(6) . . ?
C4 Ir1 C1 63.6(6) . . ?
C11 Ir1 C5 150.2(7) . . ?
C19 Ir1 C5 97.7(6) . . ?
C4 Ir1 C5 38.2(7) . . ?
C1 Ir1 C5 36.6(6) . . ?
C11 Ir1 C3 99.2(6) . . ?
C19 Ir1 C3 135.5(7) . . ?
C4 Ir1 C3 39.1(6) . . ?
C1 Ir1 C3 63.3(6) . . ?
C5 Ir1 C3 63.3(6) . . ?
C11 Ir1 C2 119.5(6) . . ?
C19 Ir1 C2 160.2(6) . . ?
C4 Ir1 C2 64.6(6) . . ?
C1 Ir1 C2 37.8(6) . . ?
C5 Ir1 C2 62.5(6) . . ?
C3 Ir1 C2 38.1(7) . . ?
C11 Ir1 Br1 87.7(5) . . ?
C19 Ir1 Br1 91.1(5) . . ?
C4 Ir1 Br1 157.9(5) . . ?
C1 Ir1 Br1 94.3(5) . . ?
C5 Ir1 Br1 122.1(5) . . ?
C3 Ir1 Br1 133.4(5) . . ?
C2 Ir1 Br1 99.1(5) . . ?
C11 N1 C12 109.9(14) . . ?
C11 N1 C24 125.4(14) . . ?
C12 N1 C24 124.2(15) . . ?
C13 N2 C11 112.3(14) . . ?
C13 N2 C14 131.7(14) . . ?
C11 N2 C14 115.5(13) . . ?
N4 N3 C21 111.0(15) . . ?
N4 N3 C17 117.7(15) . . ?
C21 N3 C17 131.4(14) . . ?
N5 N4 N3 104.3(15) . . ?
N4 N5 C20 113.7(15) . . ?
N4 N5 C22 116.4(17) . . ?
C20 N5 C22 129.6(18) . . ?

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
C5 C1 C2 C8 173.7(17) . . . . ?
C7 C1 C2 C8 0(3) . . . . ?
Ir1 C1 C2 C8 -123.2(18) . . . . ?
C5 C1 C2 C3 -3.2(19) . . . . ?
C7 C1 C2 C3 -176.7(15) . . . . ?
Ir1 C1 C2 C3 59.9(11) . . . . ?
C5 C1 C2 Ir1 -63.1(12) . . . . ?
C7 C1 C2 Ir1 123.4(16) . . . . ?
C1 C2 C3 C9 176.1(16) . . . . ?
C8 C2 C3 C9 -1(3) . . . . ?
Ir1 C2 C3 C9 -124.3(18) . . . . ?
C1 C2 C3 C4 -1.5(18) . . . . ?
C8 C2 C3 C4 -178.4(16) . . . . ?
Ir1 C2 C3 C4 58.0(11) . . . . ?
C1 C2 C3 Ir1 -59.5(12) . . . . ?
C8 C2 C3 Ir1 123.6(18) . . . . ?
C9 C3 C4 C5 -172.2(16) . . . . ?
C2 C3 C4 C5 5.5(18) . . . . ?
Ir1 C3 C4 C5 67.3(12) . . . . ?
C9 C3 C4 C10 -6(3) . . . . ?
C2 C3 C4 C10 171.7(15) . . . . ?
Ir1 C3 C4 C10 -126.5(16) . . . . ?
C9 C3 C4 Ir1 120.5(16) . . . . ?
C2 C3 C4 Ir1 -61.8(12) . . . . ?
C2 C1 C5 C4 6.7(19) . . . . ?
C7 C1 C5 C4 179.9(16) . . . . ?
Ir1 C1 C5 C4 -57.2(11) . . . . ?
C2 C1 C5 C6 -172.7(15) . . . . ?
C7 C1 C5 C6 0(3) . . . . ?
Ir1 C1 C5 C6 123.3(16) . . . . ?
C2 C1 C5 Ir1 63.9(12) . . . . ?
C7 C1 C5 Ir1 -122.9(18) . . . . ?
C3 C4 C5 C1 -7.6(19) . . . . ?
C10 C4 C5 C1 -173.0(16) . . . . ?
Ir1 C4 C5 C1 59.6(12) . . . . ?
C3 C4 C5 C6 171.9(15) . . . . ?
C10 C4 C5 C6 6(3) . . . . ?
Ir1 C4 C5 C6 -120.9(16) . . . . ?
C3 C4 C5 Ir1 -67.2(11) . . . . ?
C10 C4 C5 Ir1 127.3(18) . . . . ?
N1 C12 C13 N2 4(2) . . . . ?
N2 C14 C15 C16 178.7(17) . . . . ?
C19 C14 C15 C16 3(3) . . . . ?
C14 C15 C16 C17 -4(3) . . . . ?
C15 C16 C17 N3 180.0(17) . . . . ?
C15 C16 C17 C18 2(3) . . . . ?
C16 C17 C18 C19 1(3) . . . . ?
N3 C17 C18 C19 -176.9(16) . . . . ?
C17 C18 C19 C14 -2(2) . . . . ?
C17 C18 C19 Ir1 172.7(13) . . . . ?
C15 C14 C19 C18 0(3) . . . . ?
N2 C14 C19 C18 -176.1(15) . . . . ?
C15 C14 C19 Ir1 -175.2(15) . . . . ?
N2 C14 C19 Ir1 8.5(19) . . . . ?
N5 C20 C21 N3 -0.7(19) . . . . ?
Au1 C20 C21 N3 175.1(13) . . . . ?
N2 C11 N1 C12 1.5(19) . . . . ?
Ir1 C11 N1 C12 -178.2(15) . . . . ?
N2 C11 N1 C24 -171.0(16) . . . . ?
Ir1 C11 N1 C24 9(3) . . . . ?
C13 C12 N1 C11 -4(2) . . . . ?
C13 C12 N1 C24 168.9(17) . . . . ?
C25 C24 N1 C11 107(2) . . . . ?
C25 C24 N1 C12 -65(2) . . . . ?
C12 C13 N2 C11 -3(2) . . . . ?
C12 C13 N2 C14 -174.9(17) . . . . ?
N1 C11 N2 C13 1.2(19) . . . . ?
Ir1 C11 N2 C13 -179.0(12) . . . . ?
N1 C11 N2 C14 174.2(14) . . . . ?
Ir1 C11 N2 C14 -6.1(19) . . . . ?
C15 C14 N2 C13 -7(3) . . . . ?
C19 C14 N2 C13 169.5(17) . . . . ?
C15 C14 N2 C11 -178.1(17) . . . . ?
C19 C14 N2 C11 -2(2) . . . . ?
C20 C21 N3 N4 1(2) . . . . ?
C20 C21 N3 C17 -177.0(16) . . . . ?
C16 C17 N3 N4 -31(2) . . . . ?
C18 C17 N3 N4 146.8(16) . . . . ?
C16 C17 N3 C21 147.1(18) . . . . ?
C18 C17 N3 C21 -35(3) . . . . ?
C21 N3 N4 N5 -1.2(19) . . . . ?
C17 N3 N4 N5 177.3(14) . . . . ?
N3 N4 N5 C20 1(2) . . . . ?
N3 N4 N5 C22 175.2(15) . . . . ?
C21 C20 N5 N4 0(2) . . . . ?
Au1 C20 N5 N4 -176.1(13) . . . . ?
C21 C20 N5 C22 -173.6(18) . . . . ?
Au1 C20 N5 C22 10(3) . . . . ?
C23 C22 N5 N4 91(3) . . . . ?
C23 C22 N5 C20 -96(3) . . . . ?

_refine_diff_density_max         1.386
_refine_diff_density_min         -2.441
_refine_diff_density_rms         0.260



# start Validation Reply Form

_vrf_THETM01_mi3                 
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: Even though crystal data was collected up to 0.80 \%A resolution, 
the crystal (the largest available) still diffracted quite weakly at 
high angle.  
;
_vrf_PLAT023_mi3                 
;
PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6]..      22.15 Degree
RESPONSE: Even though crystal data was collected up to 0.80 \%A resolution, 
the crystal (the largest available) still diffracted quite weakly at 
high angle.  
;
# end Validation Reply Form
####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 2176098'
loop_
_audit_author_name
_audit_author_address
'Arnab Rit'
;IIT Madras
India
;
_audit_update_record             
;
2022-05-31 deposited with the CCDC.	2022-10-21 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         'C20 H23 Br2 N6 Pd, Br [+ solvent]'

_chemical_formula_sum            'C20 H23 Br3 N6 Pd'
_chemical_formula_weight         693.57

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

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

_cell_length_a                   19.5000(9)
_cell_length_b                   11.2281(5)
_cell_length_c                   23.8483(10)
_cell_angle_alpha                90
_cell_angle_beta                 96.656(2)
_cell_angle_gamma                90
_cell_volume                     5186.3(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)

_cell_measurement_reflns_used    3785
_cell_measurement_theta_min      2.63
_cell_measurement_theta_max      24.44
_exptl_crystal_description       BLock
_exptl_crystal_colour            colourless


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.777
_exptl_crystal_F_000             2688
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    5.356
_shelx_estimated_absorpt_T_min   0.414
_shelx_estimated_absorpt_T_max   0.616
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4928
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_process_details   'SADABS (BRuker)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a

_diffrn_source                   'fine focus sealed tube'
_diffrn_measurement_device_type  'Bruker Kappa Apex2 CCD'
_diffrn_measurement_method       'ω and φ sacn'

_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15547
_diffrn_reflns_av_unetI/netI     0.0563
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.719
_diffrn_reflns_theta_max         24.946
_diffrn_reflns_theta_full        24.946
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4548
_reflns_number_gt                3251
_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.
 
 Structure factors included contributions from the .fab file.
 
 _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 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_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)+(0.0431P)²+4.5068P] 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         4548
_refine_ls_number_parameters     293
_refine_ls_number_restraints     63
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0399
_refine_ls_wR_factor_ref         0.0923
_refine_ls_wR_factor_gt          0.0830
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_restrained_S_all      1.010
_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
Pd1 Pd 0.41971(2) 0.41122(3) 0.65528(2) 0.02711(13) Uani 1 1 d . . . . .
C1 C 0.2972(3) 0.5078(5) 0.7030(2) 0.0486(16) Uani 1 1 d . . . . .
H1 H 0.274997 0.462576 0.673631 0.058 Uiso 1 1 calc R U . . .
C2 C 0.2578(3) 0.5752(6) 0.7359(3) 0.0606(19) Uani 1 1 d . . . . .
H2 H 0.209855 0.575781 0.728744 0.073 Uiso 1 1 calc R U . . .
C3 C 0.2907(4) 0.6405(6) 0.7790(3) 0.0618(19) Uani 1 1 d . . . . .
H3 H 0.265320 0.686924 0.801419 0.074 Uiso 1 1 calc R U . . .
C4 C 0.3607(3) 0.6380(5) 0.7893(2) 0.0515(17) Uani 1 1 d . . . . .
H4 H 0.383743 0.681782 0.818794 0.062 Uiso 1 1 calc R U . . .
C5 C 0.3968(3) 0.5689(5) 0.7548(2) 0.0389(14) Uani 1 1 d . . . . .
H5 H 0.444708 0.566429 0.761782 0.047 Uiso 1 1 calc R U . . .
C6 C 0.4644(3) 0.3248(4) 0.59788(19) 0.0291(12) Uani 1 1 d . . . . .
C7 C 0.5391(3) 0.2207(5) 0.5527(2) 0.0480(16) Uani 1 1 d . . . . .
H7 H 0.578203 0.177985 0.546179 0.058 Uiso 1 1 calc R U . . .
C8 C 0.4861(3) 0.2522(5) 0.5140(2) 0.0415(15) Uani 1 1 d . . . . .
H8 H 0.481486 0.234672 0.475608 0.050 Uiso 1 1 calc R U . . .
C9 C 0.3751(3) 0.3600(4) 0.5169(2) 0.0298(12) Uani 1 1 d . . . . .
C10 C 0.3696(3) 0.4051(5) 0.4626(2) 0.0395(14) Uani 1 1 d . . . . .
H10 H 0.408287 0.408879 0.443288 0.047 Uiso 1 1 calc R U . . .
C11 C 0.3070(3) 0.4443(5) 0.4375(2) 0.0407(14) Uani 1 1 d . . . . .
H11 H 0.303004 0.474427 0.400923 0.049 Uiso 1 1 calc R U . . .
C12 C 0.2497(3) 0.4390(4) 0.4664(2) 0.0308(12) Uani 1 1 d . . . . .
C13 C 0.2544(3) 0.3930(4) 0.5199(2) 0.0337(13) Uani 1 1 d . . . . .
H13 H 0.215693 0.390014 0.539281 0.040 Uiso 1 1 calc R U . . .
C14 C 0.3172(3) 0.3512(5) 0.5449(2) 0.0309(12) Uani 1 1 d . . . . .
H14 H 0.320568 0.317047 0.580611 0.037 Uiso 1 1 calc R U . . .
C15 C 0.1215(3) 0.4780(5) 0.4591(3) 0.0485(16) Uani 1 1 d . . . . .
H15 H 0.111024 0.448679 0.493589 0.058 Uiso 1 1 calc R U . . .
C16 C 0.0778(4) 0.5272(6) 0.4178(3) 0.064(2) Uani 1 1 d . . . . .
H16 H 0.030573 0.538388 0.417611 0.077 Uiso 1 1 calc R U . . .
C17 C 0.1074(8) 0.6286(15) 0.3215(5) 0.046(4) Uani 0.498(14) 1 d D U P A 1
H17A H 0.109653 0.712935 0.330285 0.055 Uiso 0.498(14) 1 calc R U P A 1
H17B H 0.145044 0.609977 0.299737 0.055 Uiso 0.498(14) 1 calc R U P A 1
C18 C 0.0399(8) 0.6020(14) 0.2865(6) 0.090(6) Uani 0.498(14) 1 d D U P A 1
H18A H 0.036879 0.518217 0.278649 0.136 Uiso 0.498(14) 1 calc R U P A 1
H18B H 0.037358 0.645528 0.251710 0.136 Uiso 0.498(14) 1 calc R U P A 1
H18C H 0.002446 0.625335 0.306940 0.136 Uiso 0.498(14) 1 calc R U P A 1
C17' C 0.0740(8) 0.5923(17) 0.3243(6) 0.070(5) Uani 0.502(14) 1 d D U P A 2
H17C H 0.045458 0.661183 0.329613 0.084 Uiso 0.502(14) 1 calc R U P A 2
H17D H 0.045461 0.527516 0.307906 0.084 Uiso 0.502(14) 1 calc R U P A 2
C18' C 0.1311(9) 0.6206(19) 0.2911(7) 0.096(6) Uani 0.502(14) 1 d D U P A 2
H18D H 0.157315 0.686041 0.308293 0.144 Uiso 0.502(14) 1 calc R U P A 2
H18E H 0.112634 0.641871 0.253345 0.144 Uiso 0.502(14) 1 calc R U P A 2
H18F H 0.160500 0.552254 0.289970 0.144 Uiso 0.502(14) 1 calc R U P A 2
C19 C 0.5687(3) 0.2498(5) 0.6574(2) 0.0377(14) Uani 1 1 d . . . . .
H19A H 0.580612 0.166283 0.662544 0.045 Uiso 1 1 calc R U . . .
H19B H 0.544138 0.274126 0.688634 0.045 Uiso 1 1 calc R U . . .
C20 C 0.6335(3) 0.3216(6) 0.6582(2) 0.0558(17) Uani 1 1 d . . . . .
H20A H 0.660648 0.291390 0.630225 0.084 Uiso 1 1 calc R U . . .
H20B H 0.659551 0.316256 0.694799 0.084 Uiso 1 1 calc R U . . .
H20C H 0.621858 0.403374 0.649976 0.084 Uiso 1 1 calc R U . . .
N1 N 0.1163(3) 0.5567(5) 0.3769(2) 0.0605(16) Uani 1 1 d D . . . .
N2 N 0.1820(3) 0.5296(4) 0.38880(19) 0.0487(13) Uani 1 1 d . . . . .
N3 N 0.1841(2) 0.4803(4) 0.43977(18) 0.0348(11) Uani 1 1 d . . . . .
N4 N 0.4399(2) 0.3157(4) 0.54235(16) 0.0311(10) Uani 1 1 d . . . . .
N5 N 0.5235(2) 0.2648(4) 0.60418(16) 0.0358(11) Uani 1 1 d . . . . .
N6 N 0.3657(2) 0.5058(4) 0.71216(18) 0.0325(11) Uani 1 1 d . . . . .
Br1 Br 0.38189(3) 0.22092(5) 0.68890(2) 0.04358(18) Uani 1 1 d . . . . .
Br2 Br 0.46568(3) 0.59428(5) 0.62075(3) 0.04820(19) Uani 1 1 d . . . . .
Br3 Br 0.11037(3) 0.41883(5) 0.61145(2) 0.04571(18) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C6 1.962(5) . ?
Pd1 N6 2.100(4) . ?
Pd1 Br2 2.4242(7) . ?
Pd1 Br1 2.4269(7) . ?
C1 N6 1.329(7) . ?
C1 C2 1.385(8) . ?
C1 H1 0.9300 . ?
C2 C3 1.362(9) . ?
C2 H2 0.9300 . ?
C3 C4 1.358(9) . ?
C3 H3 0.9300 . ?
C4 C5 1.381(7) . ?
C4 H4 0.9300 . ?
C5 N6 1.328(6) . ?
C5 H5 0.9300 . ?
C6 N5 1.329(6) . ?
C6 N4 1.359(6) . ?
C7 C8 1.351(7) . ?
C7 N5 1.389(6) . ?
C7 H7 0.9300 . ?
C8 N4 1.385(6) . ?
C8 H8 0.9300 . ?
C9 C14 1.380(7) . ?
C9 C10 1.381(7) . ?
C9 N4 1.427(6) . ?
C10 C11 1.369(7) . ?
C10 H10 0.9300 . ?
C11 C12 1.381(7) . ?
C11 H11 0.9300 . ?
C12 C13 1.370(7) . ?
C12 N3 1.437(6) . ?
C13 C14 1.381(7) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C15 C16 1.345(8) . ?
C15 N3 1.354(7) . ?
C15 H15 0.9300 . ?
C16 N1 1.339(8) . ?
C16 H16 0.9300 . ?
C17 C18 1.503(15) . ?
C17 N1 1.540(13) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C17' N1 1.474(14) . ?
C17' C18' 1.474(16) . ?
C17' H17C 0.9700 . ?
C17' H17D 0.9700 . ?
C18' H18D 0.9600 . ?
C18' H18E 0.9600 . ?
C18' H18F 0.9600 . ?
C19 N5 1.469(6) . ?
C19 C20 1.497(8) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
N1 N2 1.315(7) . ?
N2 N3 1.332(6) . ?

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
C6 Pd1 N6 175.78(19) . . ?
C6 Pd1 Br2 88.31(15) . . ?
N6 Pd1 Br2 91.35(12) . . ?
C6 Pd1 Br1 88.39(15) . . ?
N6 Pd1 Br1 92.15(11) . . ?
Br2 Pd1 Br1 175.70(3) . . ?
N6 C1 C2 121.9(6) . . ?
N6 C1 H1 119.0 . . ?
C2 C1 H1 119.0 . . ?
C3 C2 C1 118.5(6) . . ?
C3 C2 H2 120.7 . . ?
C1 C2 H2 120.7 . . ?
C4 C3 C2 120.1(6) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C3 C4 C5 118.3(6) . . ?
C3 C4 H4 120.8 . . ?
C5 C4 H4 120.8 . . ?
N6 C5 C4 122.5(5) . . ?
N6 C5 H5 118.8 . . ?
C4 C5 H5 118.8 . . ?
N5 C6 N4 106.0(4) . . ?
N5 C6 Pd1 128.4(4) . . ?
N4 C6 Pd1 125.6(4) . . ?
C8 C7 N5 106.5(5) . . ?
C8 C7 H7 126.8 . . ?
N5 C7 H7 126.8 . . ?
C7 C8 N4 106.8(4) . . ?
C7 C8 H8 126.6 . . ?
N4 C8 H8 126.6 . . ?
C14 C9 C10 120.0(5) . . ?
C14 C9 N4 120.1(4) . . ?
C10 C9 N4 119.7(5) . . ?
C11 C10 C9 119.8(5) . . ?
C11 C10 H10 120.1 . . ?
C9 C10 H10 120.1 . . ?
C10 C11 C12 120.0(5) . . ?
C10 C11 H11 120.0 . . ?
C12 C11 H11 120.0 . . ?
C13 C12 C11 120.7(5) . . ?
C13 C12 N3 119.6(5) . . ?
C11 C12 N3 119.7(5) . . ?
C12 C13 C14 119.4(5) . . ?
C12 C13 H13 120.3 . . ?
C14 C13 H13 120.3 . . ?
C9 C14 C13 120.1(5) . . ?
C9 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
C16 C15 N3 105.1(6) . . ?
C16 C15 H15 127.4 . . ?
N3 C15 H15 127.4 . . ?
N1 C16 C15 106.0(6) . . ?
N1 C16 H16 127.0 . . ?
C15 C16 H16 127.0 . . ?
C18 C17 N1 112.1(12) . . ?
C18 C17 H17A 109.2 . . ?
N1 C17 H17A 109.2 . . ?
C18 C17 H17B 109.2 . . ?
N1 C17 H17B 109.2 . . ?
H17A C17 H17B 107.9 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N1 C17' C18' 97.6(11) . . ?
N1 C17' H17C 112.2 . . ?
C18' C17' H17C 112.2 . . ?
N1 C17' H17D 112.2 . . ?
C18' C17' H17D 112.2 . . ?
H17C C17' H17D 109.8 . . ?
C17' C18' H18D 109.5 . . ?
C17' C18' H18E 109.5 . . ?
H18D C18' H18E 109.5 . . ?
C17' C18' H18F 109.5 . . ?
H18D C18' H18F 109.5 . . ?
H18E C18' H18F 109.5 . . ?
N5 C19 C20 111.6(4) . . ?
N5 C19 H19A 109.3 . . ?
C20 C19 H19A 109.3 . . ?
N5 C19 H19B 109.3 . . ?
C20 C19 H19B 109.3 . . ?
H19A C19 H19B 108.0 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N2 N1 C16 113.5(5) . . ?
N2 N1 C17' 133.0(9) . . ?
C16 N1 C17' 112.4(9) . . ?
N2 N1 C17 108.5(8) . . ?
C16 N1 C17 137.5(8) . . ?
N1 N2 N3 102.7(5) . . ?
N2 N3 C15 112.7(5) . . ?
N2 N3 C12 118.0(5) . . ?
C15 N3 C12 129.3(5) . . ?
C6 N4 C8 109.9(4) . . ?
C6 N4 C9 125.7(4) . . ?
C8 N4 C9 124.4(4) . . ?
C6 N5 C7 110.8(4) . . ?
C6 N5 C19 125.6(4) . . ?
C7 N5 C19 123.6(4) . . ?
C5 N6 C1 118.6(5) . . ?
C5 N6 Pd1 123.1(4) . . ?
C1 N6 Pd1 118.2(4) . . ?

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
N6 C1 C2 C3 -0.4(9) . . . . ?
C1 C2 C3 C4 -0.5(10) . . . . ?
C2 C3 C4 C5 0.5(10) . . . . ?
C3 C4 C5 N6 0.4(9) . . . . ?
N5 C7 C8 N4 0.6(7) . . . . ?
C14 C9 C10 C11 1.9(8) . . . . ?
N4 C9 C10 C11 178.0(5) . . . . ?
C9 C10 C11 C12 0.3(8) . . . . ?
C10 C11 C12 C13 -1.1(8) . . . . ?
C10 C11 C12 N3 180.0(5) . . . . ?
C11 C12 C13 C14 -0.3(7) . . . . ?
N3 C12 C13 C14 178.6(4) . . . . ?
C10 C9 C14 C13 -3.3(8) . . . . ?
N4 C9 C14 C13 -179.4(4) . . . . ?
C12 C13 C14 C9 2.5(7) . . . . ?
N3 C15 C16 N1 -0.6(7) . . . . ?
C15 C16 N1 N2 0.3(7) . . . . ?
C15 C16 N1 C17' 169.8(9) . . . . ?
C15 C16 N1 C17 -170.1(10) . . . . ?
C18' C17' N1 N2 -15(2) . . . . ?
C18' C17' N1 C16 178.5(12) . . . . ?
C18 C17 N1 N2 145.3(12) . . . . ?
C18 C17 N1 C16 -44.0(19) . . . . ?
C16 N1 N2 N3 0.2(6) . . . . ?
C17' N1 N2 N3 -166.6(12) . . . . ?
C17 N1 N2 N3 173.3(7) . . . . ?
N1 N2 N3 C15 -0.5(6) . . . . ?
N1 N2 N3 C12 180.0(4) . . . . ?
C16 C15 N3 N2 0.7(6) . . . . ?
C16 C15 N3 C12 -179.9(5) . . . . ?
C13 C12 N3 N2 176.9(4) . . . . ?
C11 C12 N3 N2 -4.2(7) . . . . ?
C13 C12 N3 C15 -2.4(8) . . . . ?
C11 C12 N3 C15 176.5(5) . . . . ?
N5 C6 N4 C8 -2.0(6) . . . . ?
Pd1 C6 N4 C8 177.7(4) . . . . ?
N5 C6 N4 C9 175.6(5) . . . . ?
Pd1 C6 N4 C9 -4.8(7) . . . . ?
C7 C8 N4 C6 0.8(6) . . . . ?
C7 C8 N4 C9 -176.8(5) . . . . ?
C14 C9 N4 C6 -39.2(7) . . . . ?
C10 C9 N4 C6 144.8(5) . . . . ?
C14 C9 N4 C8 138.0(5) . . . . ?
C10 C9 N4 C8 -38.1(8) . . . . ?
N4 C6 N5 C7 2.4(6) . . . . ?
Pd1 C6 N5 C7 -177.2(4) . . . . ?
N4 C6 N5 C19 -179.9(5) . . . . ?
Pd1 C6 N5 C19 0.5(8) . . . . ?
C8 C7 N5 C6 -1.9(7) . . . . ?
C8 C7 N5 C19 -179.7(5) . . . . ?
C20 C19 N5 C6 -108.0(6) . . . . ?
C20 C19 N5 C7 69.5(7) . . . . ?
C4 C5 N6 C1 -1.3(8) . . . . ?
C4 C5 N6 Pd1 174.9(4) . . . . ?
C2 C1 N6 C5 1.2(8) . . . . ?
C2 C1 N6 Pd1 -175.1(5) . . . . ?

_refine_diff_density_max         0.728
_refine_diff_density_min         -0.527
_refine_diff_density_rms         0.106




####################################################################### 
# 
# 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_66
_database_code_depnum_ccdc_archive 'CCDC 2176100'
loop_
_audit_author_name
_audit_author_address
'Arnab Rit'
;IIT Madras
India
;
_audit_update_record             
;
2022-05-31 deposited with the CCDC.	2022-10-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C25 H27 Br4 N7 Pd2'
_chemical_formula_weight         957.97

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

_cell_length_a                   13.8366(3)
_cell_length_b                   12.6469(3)
_cell_length_c                   17.6415(4)
_cell_angle_alpha                90
_cell_angle_beta                 103.8322(9)
_cell_angle_gamma                90
_cell_volume                     2997.56(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    8163
_cell_measurement_theta_min      2.87
_cell_measurement_theta_max      27.06

_exptl_crystal_description       Rectangular
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.123
_exptl_crystal_F_000             1832
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.160
_exptl_absorpt_coefficient_mu    6.560
_shelx_estimated_absorpt_T_min   0.291
_shelx_estimated_absorpt_T_max   0.420
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.291
_exptl_absorpt_correction_T_max  0.420
_exptl_absorpt_process_details   'SADABS V2014/5(Bruker AXS.Inc)'
_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            23937
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.688
_diffrn_reflns_theta_max         24.993
_diffrn_reflns_theta_full        24.993
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5266
_reflns_number_gt                4335
_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    '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)+(0.0353P)²+9.6199P] 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         5266
_refine_ls_number_parameters     345
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0332
_refine_ls_wR_factor_ref         0.0831
_refine_ls_wR_factor_gt          0.0782
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.055
_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 -0.17166(5) 0.15962(5) 0.11480(5) 0.0490(2) Uani 1 1 d . . . . .
Br2 Br 0.17367(4) 0.21373(5) 0.24465(4) 0.03359(15) Uani 1 1 d . . . . .
Br3 Br 0.21776(4) 0.19422(5) -0.14944(3) 0.03190(15) Uani 1 1 d . . . . .
Br4 Br 0.40992(5) 0.32907(5) 0.09796(4) 0.03955(17) Uani 1 1 d . . . . .
C1 C -0.0786(4) 0.6280(5) 0.3253(3) 0.0330(13) Uani 1 1 d . . . . .
H1A H -0.0314 0.5882 0.3634 0.050 Uiso 1 1 calc R U . . .
H1B H -0.1167 0.6725 0.3513 0.050 Uiso 1 1 calc R U . . .
H1C H -0.0438 0.6708 0.2955 0.050 Uiso 1 1 calc R U . . .
C2 C -0.1466(4) 0.5539(4) 0.2721(3) 0.0233(12) Uani 1 1 d . . . . .
H2A H -0.1869 0.5162 0.3012 0.028 Uiso 1 1 calc R U . . .
H2B H -0.1909 0.5939 0.2312 0.028 Uiso 1 1 calc R U . . .
C3 C -0.0905(4) 0.3714(4) 0.2417(3) 0.0198(11) Uani 1 1 d . . . . .
H3 H -0.1257 0.3315 0.2704 0.024 Uiso 1 1 calc R U . . .
C4 C -0.0303(4) 0.3325(4) 0.1971(3) 0.0192(11) Uani 1 1 d . . . . .
C5 C 0.0664(3) 0.4351(4) 0.1157(3) 0.0153(10) Uani 1 1 d . . . . .
C6 C 0.0537(3) 0.3718(4) 0.0509(3) 0.0191(11) Uani 1 1 d . . . . .
H6 H 0.0053 0.3192 0.0420 0.023 Uiso 1 1 calc R U . . .
C7 C 0.1128(3) 0.3862(4) -0.0011(3) 0.0194(11) Uani 1 1 d . . . . .
H7 H 0.1047 0.3438 -0.0453 0.023 Uiso 1 1 calc R U . . .
C8 C 0.1843(3) 0.4650(4) 0.0138(3) 0.0171(10) Uani 1 1 d . . . . .
C9 C 0.1970(3) 0.5289(4) 0.0785(3) 0.0194(11) Uani 1 1 d . . . . .
H9 H 0.2452 0.5816 0.0873 0.023 Uiso 1 1 calc R U . . .
C10 C 0.1376(4) 0.5139(4) 0.1303(3) 0.0203(11) Uani 1 1 d . . . . .
H10 H 0.1455 0.5563 0.1745 0.024 Uiso 1 1 calc R U . . .
C11 C 0.3030(3) 0.4033(4) -0.0614(3) 0.0204(11) Uani 1 1 d . . . . .
C12 C 0.3298(4) 0.5576(4) -0.1145(3) 0.0270(12) Uani 1 1 d . . . . .
H12 H 0.3551 0.6071 -0.1436 0.032 Uiso 1 1 calc R U . . .
C13 C 0.2643(4) 0.5768(4) -0.0713(3) 0.0233(11) Uani 1 1 d . . . . .
H13 H 0.2358 0.6416 -0.0642 0.028 Uiso 1 1 calc R U . . .
C14 C 0.4234(4) 0.3993(5) -0.1467(3) 0.0328(14) Uani 1 1 d . . . . .
H14A H 0.4340 0.4444 -0.1884 0.039 Uiso 1 1 calc R U . . .
H14B H 0.3944 0.3336 -0.1700 0.039 Uiso 1 1 calc R U . . .
C15 C 0.5213(4) 0.3763(5) -0.0920(4) 0.0395(15) Uani 1 1 d . . . . .
H15A H 0.5513 0.4412 -0.0700 0.059 Uiso 1 1 calc R U . . .
H15B H 0.5641 0.3420 -0.1199 0.059 Uiso 1 1 calc R U . . .
H15C H 0.5113 0.3308 -0.0509 0.059 Uiso 1 1 calc R U . . .
C16 C -0.0121(6) -0.0222(6) 0.0916(4) 0.060(2) Uani 1 1 d . . . . .
H16 H -0.0539 0.0176 0.0529 0.072 Uiso 1 1 calc R U . . .
C17 C 0.0062(7) -0.1274(6) 0.0758(5) 0.077(3) Uani 1 1 d . . . . .
H17 H -0.0200 -0.1565 0.0268 0.093 Uiso 1 1 calc R U . . .
C18 C 0.0628(6) -0.1859(6) 0.1336(5) 0.057(2) Uani 1 1 d . . . . .
H18 H 0.0786 -0.2553 0.1240 0.069 Uiso 1 1 calc R U . . .
C19 C 0.0954(5) -0.1450(5) 0.2029(5) 0.0482(18) Uani 1 1 d . . . . .
H19 H 0.1305 -0.1864 0.2439 0.058 Uiso 1 1 calc R U . . .
C20 C 0.0771(4) -0.0390(5) 0.2149(4) 0.0383(15) Uani 1 1 d . . . . .
H20 H 0.1010 -0.0110 0.2646 0.046 Uiso 1 1 calc R U . . .
C21 C 0.2933(4) 0.0889(5) 0.0910(3) 0.0362(14) Uani 1 1 d . . . . .
H21 H 0.2644 0.1444 0.1124 0.043 Uiso 1 1 calc R U . . .
C22 C 0.3042(5) -0.0085(5) 0.1283(4) 0.0463(17) Uani 1 1 d . . . . .
H22 H 0.2820 -0.0183 0.1736 0.056 Uiso 1 1 calc R U . . .
C23 C 0.3478(5) -0.0899(5) 0.0977(4) 0.0412(15) Uani 1 1 d . . . . .
H23 H 0.3564 -0.1556 0.1221 0.049 Uiso 1 1 calc R U . . .
C24 C 0.3785(4) -0.0729(5) 0.0305(3) 0.0346(14) Uani 1 1 d . . . . .
H24 H 0.4088 -0.1268 0.0087 0.041 Uiso 1 1 calc R U . . .
C25 C 0.3640(4) 0.0252(4) -0.0042(3) 0.0289(13) Uani 1 1 d . . . . .
H25 H 0.3836 0.0357 -0.0505 0.035 Uiso 1 1 calc R U . . .
N1 N -0.0899(3) 0.4774(3) 0.2367(2) 0.0193(9) Uani 1 1 d . . . . .
N2 N -0.0338(3) 0.5119(3) 0.1915(2) 0.0206(9) Uani 1 1 d . . . . .
N3 N 0.0023(3) 0.4225(3) 0.1684(2) 0.0177(9) Uani 1 1 d . . . . .
N4 N 0.2476(3) 0.4804(3) -0.0392(2) 0.0179(9) Uani 1 1 d . . . . .
N5 N 0.3530(3) 0.4511(3) -0.1081(2) 0.0215(10) Uani 1 1 d . . . . .
N6 N 0.0284(3) 0.0233(4) 0.1602(3) 0.0305(11) Uani 1 1 d . . . . .
N7 N 0.3233(3) 0.1053(3) 0.0255(2) 0.0250(10) Uani 1 1 d . . . . .
Pd1 Pd 0.00139(3) 0.18398(3) 0.17815(2) 0.01938(11) Uani 1 1 d . . . . .
Pd2 Pd 0.31274(3) 0.25730(3) -0.02303(2) 0.02028(11) Uani 1 1 d . . . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 Pd1 2.4078(7) . ?
Br2 Pd1 2.4214(7) . ?
Br3 Pd2 2.4363(7) . ?
Br4 Pd2 2.4115(7) . ?
C1 C2 1.490(7) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 N1 1.475(6) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 N1 1.344(6) . ?
C3 C4 1.366(7) . ?
C3 H3 0.9300 . ?
C4 N3 1.366(6) . ?
C4 Pd1 1.975(5) . ?
C5 C6 1.373(7) . ?
C5 C10 1.382(7) . ?
C5 N3 1.439(6) . ?
C6 C7 1.379(7) . ?
C6 H6 0.9300 . ?
C7 C8 1.385(7) . ?
C7 H7 0.9300 . ?
C8 C9 1.375(7) . ?
C8 N4 1.439(6) . ?
C9 C10 1.381(7) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 N5 1.341(6) . ?
C11 N4 1.355(6) . ?
C11 Pd2 1.960(5) . ?
C12 C13 1.339(7) . ?
C12 N5 1.383(7) . ?
C12 H12 0.9300 . ?
C13 N4 1.386(6) . ?
C13 H13 0.9300 . ?
C14 N5 1.468(6) . ?
C14 C15 1.492(8) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 N6 1.337(8) . ?
C16 C17 1.394(10) . ?
C16 H16 0.9300 . ?
C17 C18 1.347(11) . ?
C17 H17 0.9300 . ?
C18 C19 1.306(10) . ?
C18 H18 0.9300 . ?
C19 C20 1.390(9) . ?
C19 H19 0.9300 . ?
C20 N6 1.302(7) . ?
C20 H20 0.9300 . ?
C21 N7 1.334(7) . ?
C21 C22 1.387(8) . ?
C21 H21 0.9300 . ?
C22 C23 1.368(9) . ?
C22 H22 0.9300 . ?
C23 C24 1.368(9) . ?
C23 H23 0.9300 . ?
C24 C25 1.377(8) . ?
C24 H24 0.9300 . ?
C25 N7 1.327(7) . ?
C25 H25 0.9300 . ?
N1 N2 1.313(5) . ?
N2 N3 1.339(5) . ?
N6 Pd1 2.103(5) . ?
N7 Pd2 2.095(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 C1 111.1(4) . . ?
N1 C2 H2A 109.4 . . ?
C1 C2 H2A 109.4 . . ?
N1 C2 H2B 109.4 . . ?
C1 C2 H2B 109.4 . . ?
H2A C2 H2B 108.0 . . ?
N1 C3 C4 107.9(4) . . ?
N1 C3 H3 126.0 . . ?
C4 C3 H3 126.0 . . ?
N3 C4 C3 102.4(4) . . ?
N3 C4 Pd1 128.6(4) . . ?
C3 C4 Pd1 129.1(4) . . ?
C6 C5 C10 121.3(4) . . ?
C6 C5 N3 119.9(4) . . ?
C10 C5 N3 118.8(4) . . ?
C5 C6 C7 119.9(4) . . ?
C5 C6 H6 120.0 . . ?
C7 C6 H6 120.0 . . ?
C6 C7 C8 118.7(5) . . ?
C6 C7 H7 120.7 . . ?
C8 C7 H7 120.7 . . ?
C9 C8 C7 121.6(4) . . ?
C9 C8 N4 118.9(4) . . ?
C7 C8 N4 119.5(4) . . ?
C8 C9 C10 119.4(5) . . ?
C8 C9 H9 120.3 . . ?
C10 C9 H9 120.3 . . ?
C9 C10 C5 119.1(5) . . ?
C9 C10 H10 120.5 . . ?
C5 C10 H10 120.5 . . ?
N5 C11 N4 105.3(4) . . ?
N5 C11 Pd2 129.4(4) . . ?
N4 C11 Pd2 125.1(3) . . ?
C13 C12 N5 107.9(5) . . ?
C13 C12 H12 126.1 . . ?
N5 C12 H12 126.1 . . ?
C12 C13 N4 105.9(5) . . ?
C12 C13 H13 127.0 . . ?
N4 C13 H13 127.0 . . ?
N5 C14 C15 112.8(5) . . ?
N5 C14 H14A 109.0 . . ?
C15 C14 H14A 109.0 . . ?
N5 C14 H14B 109.0 . . ?
C15 C14 H14B 109.0 . . ?
H14A C14 H14B 107.8 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N6 C16 C17 122.3(7) . . ?
N6 C16 H16 118.8 . . ?
C17 C16 H16 118.8 . . ?
C18 C17 C16 118.3(8) . . ?
C18 C17 H17 120.9 . . ?
C16 C17 H17 120.9 . . ?
C19 C18 C17 119.9(7) . . ?
C19 C18 H18 120.0 . . ?
C17 C18 H18 120.0 . . ?
C18 C19 C20 119.3(7) . . ?
C18 C19 H19 120.3 . . ?
C20 C19 H19 120.3 . . ?
N6 C20 C19 123.5(6) . . ?
N6 C20 H20 118.2 . . ?
C19 C20 H20 118.2 . . ?
N7 C21 C22 121.8(6) . . ?
N7 C21 H21 119.1 . . ?
C22 C21 H21 119.1 . . ?
C23 C22 C21 119.4(6) . . ?
C23 C22 H22 120.3 . . ?
C21 C22 H22 120.3 . . ?
C24 C23 C22 118.7(6) . . ?
C24 C23 H23 120.6 . . ?
C22 C23 H23 120.6 . . ?
C23 C24 C25 119.0(6) . . ?
C23 C24 H24 120.5 . . ?
C25 C24 H24 120.5 . . ?
N7 C25 C24 122.9(5) . . ?
N7 C25 H25 118.6 . . ?
C24 C25 H25 118.6 . . ?
N2 N1 C3 112.6(4) . . ?
N2 N1 C2 119.3(4) . . ?
C3 N1 C2 128.0(4) . . ?
N1 N2 N3 102.8(4) . . ?
N2 N3 C4 114.2(4) . . ?
N2 N3 C5 115.8(4) . . ?
C4 N3 C5 129.9(4) . . ?
C11 N4 C13 110.7(4) . . ?
C11 N4 C8 124.4(4) . . ?
C13 N4 C8 124.8(4) . . ?
C11 N5 C12 110.2(4) . . ?
C11 N5 C14 125.5(5) . . ?
C12 N5 C14 124.4(4) . . ?
C20 N6 C16 116.2(6) . . ?
C20 N6 Pd1 123.5(4) . . ?
C16 N6 Pd1 120.1(4) . . ?
C25 N7 C21 118.2(5) . . ?
C25 N7 Pd2 122.3(4) . . ?
C21 N7 Pd2 119.4(4) . . ?
C4 Pd1 N6 176.87(19) . . ?
C4 Pd1 Br1 87.93(14) . . ?
N6 Pd1 Br1 89.95(13) . . ?
C4 Pd1 Br2 90.17(14) . . ?
N6 Pd1 Br2 91.92(13) . . ?
Br1 Pd1 Br2 177.89(3) . . ?
C11 Pd2 N7 176.12(19) . . ?
C11 Pd2 Br4 85.93(14) . . ?
N7 Pd2 Br4 90.80(12) . . ?
C11 Pd2 Br3 90.84(14) . . ?
N7 Pd2 Br3 92.48(12) . . ?
Br4 Pd2 Br3 176.42(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
N1 C3 C4 N3 0.1(5) . . . . ?
N1 C3 C4 Pd1 -179.6(4) . . . . ?
C10 C5 C6 C7 0.1(7) . . . . ?
N3 C5 C6 C7 177.8(4) . . . . ?
C5 C6 C7 C8 0.1(7) . . . . ?
C6 C7 C8 C9 -0.3(7) . . . . ?
C6 C7 C8 N4 179.2(4) . . . . ?
C7 C8 C9 C10 0.4(7) . . . . ?
N4 C8 C9 C10 -179.1(4) . . . . ?
C8 C9 C10 C5 -0.2(7) . . . . ?
C6 C5 C10 C9 0.0(7) . . . . ?
N3 C5 C10 C9 -177.7(4) . . . . ?
N5 C12 C13 N4 -0.5(6) . . . . ?
N6 C16 C17 C18 3.4(14) . . . . ?
C16 C17 C18 C19 2.8(14) . . . . ?
C17 C18 C19 C20 -4.5(12) . . . . ?
C18 C19 C20 N6 0.2(10) . . . . ?
N7 C21 C22 C23 0.8(10) . . . . ?
C21 C22 C23 C24 -0.7(10) . . . . ?
C22 C23 C24 C25 -0.4(9) . . . . ?
C23 C24 C25 N7 1.5(9) . . . . ?
C4 C3 N1 N2 0.3(6) . . . . ?
C4 C3 N1 C2 177.4(4) . . . . ?
C1 C2 N1 N2 -62.2(6) . . . . ?
C1 C2 N1 C3 120.8(6) . . . . ?
C3 N1 N2 N3 -0.6(5) . . . . ?
C2 N1 N2 N3 -177.9(4) . . . . ?
N1 N2 N3 C4 0.6(5) . . . . ?
N1 N2 N3 C5 178.8(4) . . . . ?
C3 C4 N3 N2 -0.5(5) . . . . ?
Pd1 C4 N3 N2 179.2(3) . . . . ?
C3 C4 N3 C5 -178.2(4) . . . . ?
Pd1 C4 N3 C5 1.4(7) . . . . ?
C6 C5 N3 N2 -134.5(5) . . . . ?
C10 C5 N3 N2 43.3(6) . . . . ?
C6 C5 N3 C4 43.3(7) . . . . ?
C10 C5 N3 C4 -139.0(5) . . . . ?
N5 C11 N4 C13 -0.9(5) . . . . ?
Pd2 C11 N4 C13 174.3(3) . . . . ?
N5 C11 N4 C8 -177.8(4) . . . . ?
Pd2 C11 N4 C8 -2.7(7) . . . . ?
C12 C13 N4 C11 0.9(6) . . . . ?
C12 C13 N4 C8 177.8(4) . . . . ?
C9 C8 N4 C11 125.6(5) . . . . ?
C7 C8 N4 C11 -53.9(6) . . . . ?
C9 C8 N4 C13 -50.9(7) . . . . ?
C7 C8 N4 C13 129.6(5) . . . . ?
N4 C11 N5 C12 0.6(5) . . . . ?
Pd2 C11 N5 C12 -174.3(4) . . . . ?
N4 C11 N5 C14 180.0(4) . . . . ?
Pd2 C11 N5 C14 5.1(7) . . . . ?
C13 C12 N5 C11 0.0(6) . . . . ?
C13 C12 N5 C14 -179.5(5) . . . . ?
C15 C14 N5 C11 -75.5(7) . . . . ?
C15 C14 N5 C12 103.8(6) . . . . ?
C19 C20 N6 C16 5.7(9) . . . . ?
C19 C20 N6 Pd1 -179.6(5) . . . . ?
C17 C16 N6 C20 -7.4(11) . . . . ?
C17 C16 N6 Pd1 177.8(7) . . . . ?
C24 C25 N7 C21 -1.5(8) . . . . ?
C24 C25 N7 Pd2 174.7(4) . . . . ?
C22 C21 N7 C25 0.3(9) . . . . ?
C22 C21 N7 Pd2 -176.0(5) . . . . ?

_refine_diff_density_max         2.337
_refine_diff_density_min         -1.723
_refine_diff_density_rms         0.122



####################################################################### 
# 
# 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_shelx_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2176099'
loop_
_audit_author_name
_audit_author_address
'Arnab Rit'
;IIT Madras
India
;
_audit_update_record             
;
2022-05-31 deposited with the CCDC.	2022-10-21 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         'C15 H16 Br2 N4 Pd'
_chemical_formula_sum            'C15 H16 Br2 N4 Pd'
_chemical_formula_weight         518.54

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   17.7060(18)
_cell_length_b                   6.2505(7)
_cell_length_c                   15.8120(14)
_cell_angle_alpha                90
_cell_angle_beta                 98.771(3)
_cell_angle_gamma                90
_cell_volume                     1729.5(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)

_cell_measurement_reflns_used    9995
_cell_measurement_theta_min      3.01
_cell_measurement_theta_max      30.24
_exptl_crystal_description       block
_exptl_crystal_colour            yellow

_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.991
_exptl_crystal_F_000             1000
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.068
_exptl_absorpt_coefficient_mu    5.694
_shelx_estimated_absorpt_T_min   0.427
_shelx_estimated_absorpt_T_max   0.698
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5961
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   'SADABS (Bruker, 2016)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a

_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  
'Bruker D8 VENTURE diffractometer with PHOTON II detector'
_diffrn_measurement_method       'ω and φ scan'


_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            59679
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.461
_diffrn_reflns_theta_max         30.516
_diffrn_reflns_theta_full        25.242
_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             5270
_reflns_number_gt                4165
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'APEX3 (Bruker, 2016)'
_computing_cell_refinement       'APEX3/SAINT (Bruker, 2016)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2016)'

_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    
'ORTEP3 (Farrugia, 1997) and Mercury (Bruno et al., 2002)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'



_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)+(0.0277P)²+2.4420P] 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         5270
_refine_ls_number_parameters     200
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0311
_refine_ls_wR_factor_ref         0.0757
_refine_ls_wR_factor_gt          0.0670
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_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
Pd1 Pd 0.19440(2) 0.36201(3) 0.68694(2) 0.03467(6) Uani 1 1 d . . . . .
C1 C 0.34839(17) 0.6406(5) 0.6532(2) 0.0417(6) Uani 1 1 d . . . . .
H1 H 0.297343 0.651667 0.660280 0.050 Uiso 1 1 calc R U . . .
C2 C 0.39988(19) 0.8015(5) 0.6825(2) 0.0460(7) Uani 1 1 d . . . . .
H2 H 0.383250 0.920173 0.710012 0.055 Uiso 1 1 calc R U . . .
C3 C 0.47521(19) 0.7872(6) 0.6712(2) 0.0485(7) Uani 1 1 d . . . . .
H3 H 0.509236 0.896036 0.690910 0.058 Uiso 1 1 calc R U . . .
C4 C 0.50024(18) 0.6111(6) 0.6307(2) 0.0511(8) Uani 1 1 d . . . . .
H4 H 0.551068 0.602176 0.622531 0.061 Uiso 1 1 calc R U . . .
C5 C 0.44999(17) 0.4478(5) 0.6021(2) 0.0460(7) Uani 1 1 d . . . . .
H5 H 0.466986 0.328214 0.575535 0.055 Uiso 1 1 calc R U . . .
C6 C 0.37402(15) 0.4641(5) 0.61344(17) 0.0347(5) Uani 1 1 d . . . . .
C7 C 0.25264(15) 0.2391(5) 0.60231(18) 0.0368(6) Uani 1 1 d . . . . .
C8 C 0.23216(17) 0.0667(5) 0.5504(2) 0.0417(6) Uani 1 1 d . . . . .
H8 H 0.187560 -0.012944 0.548303 0.050 Uiso 1 1 calc R U . . .
C9 C 0.2907(2) -0.1333(6) 0.4372(2) 0.0514(8) Uani 1 1 d . . . . .
H9A H 0.270661 -0.265921 0.456725 0.062 Uiso 1 1 calc R U . . .
H9B H 0.257918 -0.090604 0.385112 0.062 Uiso 1 1 calc R U . . .
C10 C 0.3684(2) -0.1714(7) 0.4180(3) 0.0640(10) Uani 1 1 d . . . . .
H10A H 0.387318 -0.043349 0.395013 0.096 Uiso 1 1 calc R U . . .
H10B H 0.367186 -0.284898 0.376882 0.096 Uiso 1 1 calc R U . . .
H10C H 0.401461 -0.210868 0.469536 0.096 Uiso 1 1 calc R U . . .
C11 C 0.10004(18) 0.6798(5) 0.7746(2) 0.0470(7) Uani 1 1 d . . . . .
H11 H 0.116030 0.775874 0.736007 0.056 Uiso 1 1 calc R U . . .
C12 C 0.0502(2) 0.7493(6) 0.8277(2) 0.0573(9) Uani 1 1 d . . . . .
H12 H 0.032792 0.889876 0.824727 0.069 Uiso 1 1 calc R U . . .
C13 C 0.0266(2) 0.6085(7) 0.8853(2) 0.0605(10) Uani 1 1 d . . . . .
H13 H -0.007436 0.652112 0.921185 0.073 Uiso 1 1 calc R U . . .
C14 C 0.0540(2) 0.4030(7) 0.8889(2) 0.0578(9) Uani 1 1 d . . . . .
H14 H 0.039100 0.305025 0.927445 0.069 Uiso 1 1 calc R U . . .
C15 C 0.10411(19) 0.3446(6) 0.8344(2) 0.0478(7) Uani 1 1 d . . . . .
H15 H 0.123465 0.206011 0.837967 0.057 Uiso 1 1 calc R U . . .
N1 N 0.32173(13) 0.2963(4) 0.58065(14) 0.0344(5) Uani 1 1 d . . . . .
N2 N 0.34351(14) 0.1721(4) 0.51962(15) 0.0389(5) Uani 1 1 d . . . . .
N3 N 0.28787(14) 0.0332(4) 0.50307(15) 0.0396(5) Uani 1 1 d . . . . .
N4 N 0.12630(13) 0.4777(4) 0.77659(16) 0.0388(5) Uani 1 1 d . . . . .
Br1 Br 0.27182(2) 0.14822(7) 0.79566(2) 0.06590(12) Uani 1 1 d . . . . .
Br2 Br 0.11927(2) 0.55320(6) 0.56819(2) 0.05063(9) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C7 1.966(3) . ?
Pd1 N4 2.123(2) . ?
Pd1 Br1 2.4294(4) . ?
Pd1 Br2 2.4417(4) . ?
C1 C6 1.381(4) . ?
C1 C2 1.389(4) . ?
C1 H1 0.9300 . ?
C2 C3 1.375(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.381(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.384(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.387(4) . ?
C5 H5 0.9300 . ?
C6 N1 1.442(4) . ?
C7 N1 1.367(3) . ?
C7 C8 1.369(4) . ?
C8 N3 1.342(4) . ?
C8 H8 0.9300 . ?
C9 C10 1.474(5) . ?
C9 N3 1.478(4) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 N4 1.345(4) . ?
C11 C12 1.378(5) . ?
C11 H11 0.9300 . ?
C12 C13 1.376(6) . ?
C12 H12 0.9300 . ?
C13 C14 1.371(6) . ?
C13 H13 0.9300 . ?
C14 C15 1.376(5) . ?
C14 H14 0.9300 . ?
C15 N4 1.339(4) . ?
C15 H15 0.9300 . ?
N1 N2 1.340(3) . ?
N2 N3 1.310(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C7 Pd1 N4 176.19(11) . . ?
C7 Pd1 Br1 88.20(8) . . ?
N4 Pd1 Br1 91.80(7) . . ?
C7 Pd1 Br2 87.06(8) . . ?
N4 Pd1 Br2 92.78(7) . . ?
Br1 Pd1 Br2 174.815(16) . . ?
C6 C1 C2 119.1(3) . . ?
C6 C1 H1 120.5 . . ?
C2 C1 H1 120.5 . . ?
C3 C2 C1 120.7(3) . . ?
C3 C2 H2 119.7 . . ?
C1 C2 H2 119.7 . . ?
C2 C3 C4 119.9(3) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C3 C4 C5 120.2(3) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
C4 C5 C6 119.5(3) . . ?
C4 C5 H5 120.3 . . ?
C6 C5 H5 120.3 . . ?
C1 C6 C5 120.7(3) . . ?
C1 C6 N1 120.5(2) . . ?
C5 C6 N1 118.8(3) . . ?
N1 C7 C8 102.8(2) . . ?
N1 C7 Pd1 130.6(2) . . ?
C8 C7 Pd1 126.7(2) . . ?
N3 C8 C7 107.9(3) . . ?
N3 C8 H8 126.1 . . ?
C7 C8 H8 126.1 . . ?
C10 C9 N3 113.1(3) . . ?
C10 C9 H9A 109.0 . . ?
N3 C9 H9A 109.0 . . ?
C10 C9 H9B 109.0 . . ?
N3 C9 H9B 109.0 . . ?
H9A C9 H9B 107.8 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N4 C11 C12 122.2(3) . . ?
N4 C11 H11 118.9 . . ?
C12 C11 H11 118.9 . . ?
C13 C12 C11 119.3(3) . . ?
C13 C12 H12 120.4 . . ?
C11 C12 H12 120.4 . . ?
C14 C13 C12 119.1(3) . . ?
C14 C13 H13 120.5 . . ?
C12 C13 H13 120.5 . . ?
C13 C14 C15 118.7(4) . . ?
C13 C14 H14 120.7 . . ?
C15 C14 H14 120.7 . . ?
N4 C15 C14 123.2(3) . . ?
N4 C15 H15 118.4 . . ?
C14 C15 H15 118.4 . . ?
N2 N1 C7 113.3(2) . . ?
N2 N1 C6 116.1(2) . . ?
C7 N1 C6 130.5(2) . . ?
N3 N2 N1 103.7(2) . . ?
N2 N3 C8 112.3(2) . . ?
N2 N3 C9 120.2(3) . . ?
C8 N3 C9 127.5(3) . . ?
C15 N4 C11 117.6(3) . . ?
C15 N4 Pd1 120.0(2) . . ?
C11 N4 Pd1 122.2(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 0.8(5) . . . . ?
C1 C2 C3 C4 -0.2(5) . . . . ?
C2 C3 C4 C5 -0.7(6) . . . . ?
C3 C4 C5 C6 0.9(5) . . . . ?
C2 C1 C6 C5 -0.5(5) . . . . ?
C2 C1 C6 N1 -178.7(3) . . . . ?
C4 C5 C6 C1 -0.3(5) . . . . ?
C4 C5 C6 N1 177.8(3) . . . . ?
N1 C7 C8 N3 0.0(3) . . . . ?
Pd1 C7 C8 N3 -179.2(2) . . . . ?
N4 C11 C12 C13 0.3(6) . . . . ?
C11 C12 C13 C14 0.8(6) . . . . ?
C12 C13 C14 C15 -0.3(6) . . . . ?
C13 C14 C15 N4 -1.4(6) . . . . ?
C8 C7 N1 N2 0.4(3) . . . . ?
Pd1 C7 N1 N2 179.6(2) . . . . ?
C8 C7 N1 C6 -178.7(3) . . . . ?
Pd1 C7 N1 C6 0.5(5) . . . . ?
C1 C6 N1 N2 158.1(3) . . . . ?
C5 C6 N1 N2 -20.0(4) . . . . ?
C1 C6 N1 C7 -22.8(4) . . . . ?
C5 C6 N1 C7 159.1(3) . . . . ?
C7 N1 N2 N3 -0.6(3) . . . . ?
C6 N1 N2 N3 178.6(2) . . . . ?
N1 N2 N3 C8 0.6(3) . . . . ?
N1 N2 N3 C9 179.5(3) . . . . ?
C7 C8 N3 N2 -0.4(4) . . . . ?
C7 C8 N3 C9 -179.2(3) . . . . ?
C10 C9 N3 N2 20.2(5) . . . . ?
C10 C9 N3 C8 -161.1(3) . . . . ?
C14 C15 N4 C11 2.5(5) . . . . ?
C14 C15 N4 Pd1 -173.5(3) . . . . ?
C12 C11 N4 C15 -1.9(5) . . . . ?
C12 C11 N4 Pd1 174.0(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C8 H8 Br2 0.93 3.01 3.814(3) 146.4 1_545 yes
C9 H9B Br1 0.97 3.13 3.753(4) 123.3 4_565 yes
C10 H10B Br1 0.96 3.00 3.813(4) 143.4 4 yes
C15 H15 Br1 0.93 2.83 3.355(3) 116.8 . yes

_refine_diff_density_max         0.894
_refine_diff_density_min         -1.469
_refine_diff_density_rms         0.089



####################################################################### 
# 
# 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_13
_database_code_depnum_ccdc_archive 'CCDC 2176104'
loop_
_audit_author_name
_audit_author_address
'Arnab Rit'
;IIT Madras
India
;
_audit_update_record             
;
2022-05-31 deposited with the CCDC.	2022-10-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H21 Br2 N5 O'
_chemical_formula_sum            'C15 H21 Br2 N5 O'
_chemical_formula_weight         447.19

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

_cell_length_a                   7.7483(3)
_cell_length_b                   23.2239(11)
_cell_length_c                   10.3010(5)
_cell_angle_alpha                90
_cell_angle_beta                 102.9736(17)
_cell_angle_gamma                90
_cell_volume                     1806.30(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4215
_cell_measurement_theta_min      2.63
_cell_measurement_theta_max      26.13

_exptl_crystal_description       Rectangular
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_F_000             896
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.160
_exptl_absorpt_coefficient_mu    4.499
_shelx_estimated_absorpt_T_min   0.399
_shelx_estimated_absorpt_T_max   0.533
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.399
_exptl_absorpt_correction_T_max  0.533
_exptl_absorpt_process_details   'SADABS V2014/5(Bruker AXS.Inc)'
_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            10998
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.754
_diffrn_reflns_theta_max         24.987
_diffrn_reflns_theta_full        24.987
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measured_fraction_theta_full 0.952
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_Laue_measured_fraction_full 0.952
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_point_group_measured_fraction_full 0.952
_reflns_number_total             3025
_reflns_number_gt                2468
_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    '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)+(0.0195P)²+3.1479P] 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     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3025
_refine_ls_number_parameters     218
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0390
_refine_ls_wR_factor_ref         0.0752
_refine_ls_wR_factor_gt          0.0714
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_restrained_S_all      1.111
_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 0.28784(6) 0.06238(2) 0.53576(5) 0.04884(15) Uani 1 1 d . . . . .
Br2 Br 0.58856(6) 0.25744(2) 0.42287(4) 0.04526(14) Uani 1 1 d . . . . .
C1 C 0.2062(7) -0.1089(2) 0.4621(5) 0.0612(14) Uani 1 1 d . . . . .
H1A H 0.2855 -0.0776 0.4932 0.092 Uiso 1 1 calc R U . . .
H1B H 0.2190 -0.1379 0.5302 0.092 Uiso 1 1 calc R U . . .
H1C H 0.0864 -0.0951 0.4415 0.092 Uiso 1 1 calc R U . . .
C2 C 0.2486(7) -0.13392(18) 0.3418(4) 0.0562(13) Uani 1 1 d . . . . .
H2A H 0.1691 -0.1659 0.3117 0.067 Uiso 1 1 calc R U . . .
H2B H 0.3684 -0.1489 0.3641 0.067 Uiso 1 1 calc R U . . .
C3 C 0.1460(5) -0.10004(17) 0.1025(4) 0.0377(10) Uani 1 1 d . . . . .
H3 H 0.0791 -0.1321 0.0687 0.045 Uiso 1 1 calc R U . . .
C4 C 0.1740(5) -0.05360(16) 0.0333(4) 0.0367(10) Uani 1 1 d . . . . .
H4 H 0.1311 -0.0475 -0.0574 0.044 Uiso 1 1 calc R U . . .
C5 C 0.3114(5) -0.04090(16) 0.2408(4) 0.0383(10) Uani 1 1 d . . . . .
H5 H 0.3789 -0.0249 0.3185 0.046 Uiso 1 1 calc R U . . .
C6 C 0.3453(5) 0.03870(15) 0.0913(4) 0.0273(8) Uani 1 1 d . . . . .
C7 C 0.3174(5) 0.05683(17) -0.0383(4) 0.0385(10) Uani 1 1 d . . . . .
H7 H 0.2559 0.0335 -0.1066 0.046 Uiso 1 1 calc R U . . .
C8 C 0.3806(5) 0.10977(16) -0.0676(4) 0.0388(10) Uani 1 1 d . . . . .
H8 H 0.3614 0.1224 -0.1553 0.047 Uiso 1 1 calc R U . . .
C9 C 0.4716(5) 0.14343(15) 0.0337(4) 0.0285(9) Uani 1 1 d . . . . .
C10 C 0.5004(6) 0.12590(17) 0.1634(4) 0.0415(11) Uani 1 1 d . . . . .
H10 H 0.5629 0.1493 0.2312 0.050 Uiso 1 1 calc R U . . .
C11 C 0.4358(6) 0.07296(17) 0.1934(4) 0.0429(11) Uani 1 1 d . . . . .
H11 H 0.4533 0.0607 0.2814 0.051 Uiso 1 1 calc R U . . .
C12 C 0.6419(6) 0.28423(18) 0.0113(4) 0.0434(11) Uani 1 1 d . . . . .
H12 H 0.6871 0.3204 0.0393 0.052 Uiso 1 1 calc R U . . .
C13 C 0.5944(5) 0.24245(17) 0.0874(4) 0.0398(10) Uani 1 1 d . . . . .
H13 H 0.5993 0.2438 0.1784 0.048 Uiso 1 1 calc R U . . .
C14 C 0.6406(7) 0.2915(2) -0.2317(5) 0.0557(13) Uani 1 1 d . . . . .
H14A H 0.7639 0.3029 -0.2168 0.067 Uiso 1 1 calc R U . . .
H14B H 0.6175 0.2642 -0.3048 0.067 Uiso 1 1 calc R U . . .
C15 C 0.5306(9) 0.3415(2) -0.2692(6) 0.0816(18) Uani 1 1 d . . . . .
H15A H 0.4090 0.3298 -0.2966 0.122 Uiso 1 1 calc R U . . .
H15B H 0.5655 0.3609 -0.3416 0.122 Uiso 1 1 calc R U . . .
H15C H 0.5440 0.3671 -0.1945 0.122 Uiso 1 1 calc R U . . .
N1 N 0.2335(5) -0.09180(13) 0.2318(3) 0.0388(8) Uani 1 1 d . . . . .
N2 N 0.2785(4) -0.01634(12) 0.1221(3) 0.0280(7) Uani 1 1 d . . . . .
N3 N 0.5385(4) 0.19838(13) 0.0039(3) 0.0298(7) Uani 1 1 d . . . . .
N4 N 0.5475(4) 0.21036(14) -0.1190(3) 0.0374(8) Uani 1 1 d . . . . .
N5 N 0.6109(4) 0.26323(14) -0.1117(3) 0.0382(8) Uani 1 1 d . . . . .
O1 O 0.9438(6) 0.01750(17) 0.2870(4) 0.0676(10) Uani 1 1 d D . . . .
H2O H 1.029(5) 0.031(2) 0.344(4) 0.09(2) Uiso 1 1 d D . . . .
H1O H 0.881(6) -0.0040(18) 0.325(4) 0.063(17) Uiso 1 1 d D . . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.470(6) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 N1 1.481(5) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.337(5) . ?
C3 N1 1.366(5) . ?
C3 H3 0.9300 . ?
C4 N2 1.381(5) . ?
C4 H4 0.9300 . ?
C5 N2 1.321(5) . ?
C5 N1 1.321(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.371(5) . ?
C6 C11 1.378(5) . ?
C6 N2 1.441(4) . ?
C7 C8 1.381(5) . ?
C7 H7 0.9300 . ?
C8 C9 1.366(5) . ?
C8 H8 0.9300 . ?
C9 C10 1.366(5) . ?
C9 N3 1.436(5) . ?
C10 C11 1.388(5) . ?
C10 H10 0.9300 . ?
C11 H11 0.9300 . ?
C12 N5 1.329(5) . ?
C12 C13 1.349(6) . ?
C12 H12 0.9300 . ?
C13 N3 1.345(5) . ?
C13 H13 0.9300 . ?
C14 C15 1.441(7) . ?
C14 N5 1.463(5) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
N3 N4 1.314(4) . ?
N4 N5 1.318(4) . ?
O1 H2O 0.84(2) . ?
O1 H1O 0.847(19) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C1 C2 N1 112.9(4) . . ?
C1 C2 H2A 109.0 . . ?
N1 C2 H2A 109.0 . . ?
C1 C2 H2B 109.0 . . ?
N1 C2 H2B 109.0 . . ?
H2A C2 H2B 107.8 . . ?
C4 C3 N1 107.6(3) . . ?
C4 C3 H3 126.2 . . ?
N1 C3 H3 126.2 . . ?
C3 C4 N2 107.1(3) . . ?
C3 C4 H4 126.5 . . ?
N2 C4 H4 126.5 . . ?
N2 C5 N1 109.4(3) . . ?
N2 C5 H5 125.3 . . ?
N1 C5 H5 125.3 . . ?
C7 C6 C11 120.6(3) . . ?
C7 C6 N2 120.1(3) . . ?
C11 C6 N2 119.4(3) . . ?
C6 C7 C8 120.0(4) . . ?
C6 C7 H7 120.0 . . ?
C8 C7 H7 120.0 . . ?
C9 C8 C7 119.4(4) . . ?
C9 C8 H8 120.3 . . ?
C7 C8 H8 120.3 . . ?
C8 C9 C10 121.3(4) . . ?
C8 C9 N3 119.6(3) . . ?
C10 C9 N3 119.1(3) . . ?
C9 C10 C11 119.6(4) . . ?
C9 C10 H10 120.2 . . ?
C11 C10 H10 120.2 . . ?
C6 C11 C10 119.2(4) . . ?
C6 C11 H11 120.4 . . ?
C10 C11 H11 120.4 . . ?
N5 C12 C13 106.0(4) . . ?
N5 C12 H12 127.0 . . ?
C13 C12 H12 127.0 . . ?
N3 C13 C12 105.5(4) . . ?
N3 C13 H13 127.3 . . ?
C12 C13 H13 127.3 . . ?
C15 C14 N5 113.1(4) . . ?
C15 C14 H14A 109.0 . . ?
N5 C14 H14A 109.0 . . ?
C15 C14 H14B 109.0 . . ?
N5 C14 H14B 109.0 . . ?
H14A C14 H14B 107.8 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C5 N1 C3 108.2(3) . . ?
C5 N1 C2 125.5(4) . . ?
C3 N1 C2 126.2(3) . . ?
C5 N2 C4 107.7(3) . . ?
C5 N2 C6 125.6(3) . . ?
C4 N2 C6 126.6(3) . . ?
N4 N3 C13 112.1(3) . . ?
N4 N3 C9 119.6(3) . . ?
C13 N3 C9 128.3(3) . . ?
N3 N4 N5 104.0(3) . . ?
N4 N5 C12 112.5(3) . . ?
N4 N5 C14 119.8(4) . . ?
C12 N5 C14 127.8(4) . . ?
H2O O1 H1O 110(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
N1 C3 C4 N2 -0.6(5) . . . . ?
C11 C6 C7 C8 0.2(6) . . . . ?
N2 C6 C7 C8 179.6(4) . . . . ?
C6 C7 C8 C9 0.4(6) . . . . ?
C7 C8 C9 C10 -0.4(6) . . . . ?
C7 C8 C9 N3 179.7(4) . . . . ?
C8 C9 C10 C11 -0.2(6) . . . . ?
N3 C9 C10 C11 179.8(4) . . . . ?
C7 C6 C11 C10 -0.7(6) . . . . ?
N2 C6 C11 C10 179.8(4) . . . . ?
C9 C10 C11 C6 0.7(6) . . . . ?
N5 C12 C13 N3 0.4(5) . . . . ?
N2 C5 N1 C3 -0.5(5) . . . . ?
N2 C5 N1 C2 176.0(4) . . . . ?
C4 C3 N1 C5 0.7(5) . . . . ?
C4 C3 N1 C2 -175.8(4) . . . . ?
C1 C2 N1 C5 52.8(6) . . . . ?
C1 C2 N1 C3 -131.4(5) . . . . ?
N1 C5 N2 C4 0.1(4) . . . . ?
N1 C5 N2 C6 -178.1(3) . . . . ?
C3 C4 N2 C5 0.3(4) . . . . ?
C3 C4 N2 C6 178.5(3) . . . . ?
C7 C6 N2 C5 173.0(4) . . . . ?
C11 C6 N2 C5 -7.6(6) . . . . ?
C7 C6 N2 C4 -4.9(5) . . . . ?
C11 C6 N2 C4 174.5(4) . . . . ?
C12 C13 N3 N4 -0.3(5) . . . . ?
C12 C13 N3 C9 -179.3(4) . . . . ?
C8 C9 N3 N4 -15.2(5) . . . . ?
C10 C9 N3 N4 164.8(4) . . . . ?
C8 C9 N3 C13 163.7(4) . . . . ?
C10 C9 N3 C13 -16.3(6) . . . . ?
C13 N3 N4 N5 0.1(4) . . . . ?
C9 N3 N4 N5 179.1(3) . . . . ?
N3 N4 N5 C12 0.2(4) . . . . ?
N3 N4 N5 C14 179.7(3) . . . . ?
C13 C12 N5 N4 -0.4(5) . . . . ?
C13 C12 N5 C14 -179.8(4) . . . . ?
C15 C14 N5 N4 116.0(5) . . . . ?
C15 C14 N5 C12 -64.7(6) . . . . ?

_refine_diff_density_max         0.516
_refine_diff_density_min         -0.354
_refine_diff_density_rms         0.068



####################################################################### 
# 
# 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_shelx_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 2176102'
loop_
_audit_author_name
_audit_author_address
'Arnab Rit'
;IIT Madras
India
;
_audit_update_record             
;
2022-05-31 deposited with the CCDC.	2022-10-21 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         'C20 H22 Au Br2.59 Cl0.41 N6 Pd'

_chemical_formula_sum            'C20 H22 Au Br2.59 Cl0.41 N6 Pd'
_chemical_formula_weight         871.30

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.2856(4)
_cell_length_b                   12.0023(6)
_cell_length_c                   12.6741(6)
_cell_angle_alpha                83.517(2)
_cell_angle_beta                 83.226(2)
_cell_angle_gamma                88.824(2)
_cell_volume                     1243.56(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    200(2)

_cell_measurement_reflns_used    9729
_cell_measurement_theta_min      3.00
_cell_measurement_theta_max      31.51
_exptl_crystal_description       BLOCK
_exptl_crystal_colour            YELLOW



_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.327
_exptl_crystal_F_000             813
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    10.840
_shelx_estimated_absorpt_T_min   0.293
_shelx_estimated_absorpt_T_max   0.410
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3425
_exptl_absorpt_correction_T_max  0.6842
_exptl_absorpt_process_details   'SADABS (Bruker, 2016)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a

_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  
'Bruker D8 VENTURE diffractometer with PHOTON II detector'
_diffrn_measurement_method       'ω and φ scan'



_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            51560
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.800
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_full        24.998
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             4327
_reflns_number_gt                4057
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'APEX3 (Bruker, 2016)'
_computing_cell_refinement       'APEX3/SAINT (Bruker, 2016)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2016)'

_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    
'ORTEP3 (Farrugia, 1997) and Mercury (Bruno et al., 2002)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'


_refine_special_details          
;
the crystal lattice contains two types of molecules with Br and Cl
attached to Au with a ratio of 59:41 respectively
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0418P)²+11.5644P] 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         4327
_refine_ls_number_parameters     290
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0310
_refine_ls_wR_factor_ref         0.0920
_refine_ls_wR_factor_gt          0.0881
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.057
_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
Pd1 Pd 0.31326(6) 0.21978(4) 0.39693(4) 0.02276(13) Uani 1 1 d . . . . .
Au1 Au 0.26531(3) 0.40710(2) -0.06249(2) 0.03143(11) Uani 1 1 d . . . . .
C1 C 0.2196(9) -0.0138(6) 0.3669(6) 0.0376(17) Uani 1 1 d . . . . .
H1 H 0.172199 -0.013660 0.438918 0.045 Uiso 1 1 calc R U . . .
C2 C 0.2065(10) -0.1078(6) 0.3152(7) 0.0424(18) Uani 1 1 d . . . . .
H2 H 0.150904 -0.172044 0.351475 0.051 Uiso 1 1 calc R U . . .
C3 C 0.2741(10) -0.1078(7) 0.2114(7) 0.0439(19) Uani 1 1 d . . . . .
H3 H 0.264958 -0.171729 0.174651 0.053 Uiso 1 1 calc R U . . .
C4 C 0.3550(10) -0.0147(7) 0.1612(6) 0.0420(18) Uani 1 1 d . . . . .
H4 H 0.403155 -0.013472 0.089189 0.050 Uiso 1 1 calc R U . . .
C5 C 0.3659(9) 0.0771(6) 0.2160(6) 0.0338(16) Uani 1 1 d . . . . .
H5 H 0.422704 0.141438 0.180993 0.041 Uiso 1 1 calc R U . . .
C6 C 0.3187(8) 0.3489(6) 0.4783(5) 0.0253(13) Uani 1 1 d . . . . .
C7 C 0.3231(9) 0.4504(6) 0.6156(6) 0.0332(16) Uani 1 1 d . . . . .
H7 H 0.335183 0.469001 0.685155 0.040 Uiso 1 1 calc R U . . .
C8 C 0.2794(8) 0.5210(6) 0.5341(6) 0.0300(15) Uani 1 1 d . . . . .
H8 H 0.254241 0.598513 0.534560 0.036 Uiso 1 1 calc R U . . .
C9 C 0.2491(7) 0.5005(5) 0.3432(5) 0.0221(12) Uani 1 1 d . . . . .
C10 C 0.1205(8) 0.5739(5) 0.3272(5) 0.0275(14) Uani 1 1 d . . . . .
H10 H 0.051929 0.596985 0.386425 0.033 Uiso 1 1 calc R U . . .
C11 C 0.0935(8) 0.6130(6) 0.2233(6) 0.0290(14) Uani 1 1 d . . . . .
H11 H 0.005063 0.662515 0.210953 0.035 Uiso 1 1 calc R U . . .
C12 C 0.1949(8) 0.5800(5) 0.1382(5) 0.0254(13) Uani 1 1 d . . . . .
C13 C 0.3252(8) 0.5079(6) 0.1545(5) 0.0261(13) Uani 1 1 d . . . . .
H13 H 0.395903 0.486709 0.095364 0.031 Uiso 1 1 calc R U . . .
C14 C 0.3507(8) 0.4674(5) 0.2576(5) 0.0252(13) Uani 1 1 d . . . . .
H14 H 0.438012 0.416865 0.269726 0.030 Uiso 1 1 calc R U . . .
C15 C 0.1307(9) 0.6430(6) -0.1352(6) 0.0360(16) Uani 1 1 d . . . . .
H15 H 0.124053 0.633893 -0.208059 0.043 Uiso 1 1 calc R U . . .
C16 C 0.1845(8) 0.5636(6) -0.0590(5) 0.0296(14) Uani 1 1 d . . . . .
C17 C 0.0241(13) 0.8431(7) -0.1354(7) 0.057(3) Uani 1 1 d . . . . .
H17A H 0.018350 0.839247 -0.212451 0.068 Uiso 1 1 calc R U . . .
H17B H -0.087248 0.855738 -0.100857 0.068 Uiso 1 1 calc R U . . .
C18 C 0.1286(17) 0.9370(9) -0.1220(14) 0.105(6) Uani 1 1 d . . . . .
H18A H 0.083884 1.007172 -0.154327 0.158 Uiso 1 1 calc R U . . .
H18B H 0.132957 0.941337 -0.045620 0.158 Uiso 1 1 calc R U . . .
H18C H 0.238387 0.924872 -0.157035 0.158 Uiso 1 1 calc R U . . .
C19 C 0.4070(10) 0.2466(7) 0.6441(6) 0.0427(19) Uani 1 1 d . . . . .
H19A H 0.446015 0.269795 0.709121 0.051 Uiso 1 1 calc R U . . .
H19B H 0.500378 0.213809 0.601627 0.051 Uiso 1 1 calc R U . . .
C20 C 0.2784(14) 0.1585(8) 0.6765(8) 0.062(3) Uani 1 1 d . . . . .
H20A H 0.324064 0.094239 0.718331 0.093 Uiso 1 1 calc R U . . .
H20B H 0.186619 0.189875 0.719969 0.093 Uiso 1 1 calc R U . . .
H20C H 0.240993 0.133878 0.612454 0.093 Uiso 1 1 calc R U . . .
N1 N 0.2991(7) 0.0782(5) 0.3167(5) 0.0299(12) Uani 1 1 d . . . . .
N2 N 0.2783(6) 0.4576(4) 0.4486(4) 0.0232(11) Uani 1 1 d . . . . .
N3 N 0.3474(7) 0.3459(5) 0.5809(4) 0.0290(12) Uani 1 1 d . . . . .
N4 N 0.1658(7) 0.6195(5) 0.0319(4) 0.0269(12) Uani 1 1 d . . . . .
N5 N 0.1091(8) 0.7243(5) 0.0151(5) 0.0354(14) Uani 1 1 d . . . . .
N6 N 0.0894(8) 0.7356(6) -0.0869(5) 0.0396(15) Uani 1 1 d . . . . .
Br2 Br 0.02161(9) 0.23567(7) 0.42091(7) 0.0449(2) Uani 1 1 d . . . . .
Br3 Br 0.60558(10) 0.21089(8) 0.37132(8) 0.0540(2) Uani 1 1 d . . . . .
Br1 Br 0.3783(12) 0.2227(7) -0.0574(7) 0.0545(15) Uani 0.592(9) 1 d . . P A 1
Cl1 Cl 0.337(4) 0.228(3) -0.064(3) 0.066(8) Uani 0.408(9) 1 d . . P A 2


_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
Pd1 C6 1.960(7) . ?
Pd1 N1 2.089(6) . ?
Pd1 Br2 2.4061(9) . ?
Pd1 Br3 2.4072(10) . ?
Au1 C16 1.984(7) . ?
Au1 Cl1 2.22(3) . ?
Au1 Br1 2.382(9) . ?
C1 N1 1.353(9) . ?
C1 C2 1.379(11) . ?
C1 H1 0.9500 . ?
C2 C3 1.368(12) . ?
C2 H2 0.9500 . ?
C3 C4 1.369(12) . ?
C3 H3 0.9500 . ?
C4 C5 1.378(11) . ?
C4 H4 0.9500 . ?
C5 N1 1.331(9) . ?
C5 H5 0.9500 . ?
C6 N3 1.346(9) . ?
C6 N2 1.363(9) . ?
C7 C8 1.340(11) . ?
C7 N3 1.379(9) . ?
C7 H7 0.9500 . ?
C8 N2 1.394(8) . ?
C8 H8 0.9500 . ?
C9 C14 1.382(9) . ?
C9 C10 1.387(9) . ?
C9 N2 1.422(8) . ?
C10 C11 1.390(10) . ?
C10 H10 0.9500 . ?
C11 C12 1.376(10) . ?
C11 H11 0.9500 . ?
C12 C13 1.389(9) . ?
C12 N4 1.424(8) . ?
C13 C14 1.380(9) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 N6 1.348(10) . ?
C15 C16 1.385(10) . ?
C15 H15 0.9500 . ?
C16 N4 1.389(9) . ?
C17 C18 1.471(17) . ?
C17 N6 1.485(10) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 N3 1.469(9) . ?
C19 C20 1.505(13) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
N4 N5 1.337(8) . ?
N5 N6 1.314(9) . ?

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
C6 Pd1 N1 177.0(2) . . ?
C6 Pd1 Br2 87.50(18) . . ?
N1 Pd1 Br2 90.68(16) . . ?
C6 Pd1 Br3 91.09(18) . . ?
N1 Pd1 Br3 90.79(16) . . ?
Br2 Pd1 Br3 177.99(4) . . ?
C16 Au1 Cl1 175.9(9) . . ?
C16 Au1 Br1 175.3(3) . . ?
N1 C1 C2 121.0(7) . . ?
N1 C1 H1 119.5 . . ?
C2 C1 H1 119.5 . . ?
C3 C2 C1 119.5(7) . . ?
C3 C2 H2 120.2 . . ?
C1 C2 H2 120.2 . . ?
C2 C3 C4 119.2(7) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C3 C4 C5 119.3(7) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 H4 120.3 . . ?
N1 C5 C4 121.8(7) . . ?
N1 C5 H5 119.1 . . ?
C4 C5 H5 119.1 . . ?
N3 C6 N2 105.1(6) . . ?
N3 C6 Pd1 126.3(5) . . ?
N2 C6 Pd1 128.2(5) . . ?
C8 C7 N3 108.0(6) . . ?
C8 C7 H7 126.0 . . ?
N3 C7 H7 126.0 . . ?
C7 C8 N2 106.1(6) . . ?
C7 C8 H8 127.0 . . ?
N2 C8 H8 127.0 . . ?
C14 C9 C10 121.0(6) . . ?
C14 C9 N2 118.8(6) . . ?
C10 C9 N2 120.3(6) . . ?
C9 C10 C11 119.0(6) . . ?
C9 C10 H10 120.5 . . ?
C11 C10 H10 120.5 . . ?
C12 C11 C10 120.0(6) . . ?
C12 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
C11 C12 C13 121.0(6) . . ?
C11 C12 N4 119.7(6) . . ?
C13 C12 N4 119.3(6) . . ?
C14 C13 C12 119.2(6) . . ?
C14 C13 H13 120.4 . . ?
C12 C13 H13 120.4 . . ?
C13 C14 C9 120.0(6) . . ?
C13 C14 H14 120.0 . . ?
C9 C14 H14 120.0 . . ?
N6 C15 C16 107.3(6) . . ?
N6 C15 H15 126.3 . . ?
C16 C15 H15 126.3 . . ?
C15 C16 N4 102.2(6) . . ?
C15 C16 Au1 133.5(6) . . ?
N4 C16 Au1 124.3(5) . . ?
C18 C17 N6 110.5(8) . . ?
C18 C17 H17A 109.6 . . ?
N6 C17 H17A 109.6 . . ?
C18 C17 H17B 109.6 . . ?
N6 C17 H17B 109.6 . . ?
H17A C17 H17B 108.1 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N3 C19 C20 112.7(7) . . ?
N3 C19 H19A 109.1 . . ?
C20 C19 H19A 109.1 . . ?
N3 C19 H19B 109.1 . . ?
C20 C19 H19B 109.1 . . ?
H19A C19 H19B 107.8 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C5 N1 C1 119.1(6) . . ?
C5 N1 Pd1 121.0(5) . . ?
C1 N1 Pd1 119.9(5) . . ?
C6 N2 C8 110.3(5) . . ?
C6 N2 C9 124.2(5) . . ?
C8 N2 C9 125.4(6) . . ?
C6 N3 C7 110.5(6) . . ?
C6 N3 C19 124.3(6) . . ?
C7 N3 C19 125.0(6) . . ?
N5 N4 C16 113.8(6) . . ?
N5 N4 C12 117.0(5) . . ?
C16 N4 C12 129.2(6) . . ?
N6 N5 N4 103.4(6) . . ?
N5 N6 C15 113.3(6) . . ?
N5 N6 C17 119.1(7) . . ?
C15 N6 C17 127.6(7) . . ?

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
N1 C1 C2 C3 -0.3(12) . . . . ?
C1 C2 C3 C4 0.6(13) . . . . ?
C2 C3 C4 C5 -0.3(13) . . . . ?
C3 C4 C5 N1 -0.3(12) . . . . ?
N3 C7 C8 N2 -0.3(8) . . . . ?
C14 C9 C10 C11 0.8(10) . . . . ?
N2 C9 C10 C11 -179.0(6) . . . . ?
C9 C10 C11 C12 -0.8(10) . . . . ?
C10 C11 C12 C13 -0.2(10) . . . . ?
C10 C11 C12 N4 179.4(6) . . . . ?
C11 C12 C13 C14 1.3(10) . . . . ?
N4 C12 C13 C14 -178.3(6) . . . . ?
C12 C13 C14 C9 -1.3(10) . . . . ?
C10 C9 C14 C13 0.3(10) . . . . ?
N2 C9 C14 C13 -179.9(6) . . . . ?
N6 C15 C16 N4 1.1(8) . . . . ?
N6 C15 C16 Au1 179.7(5) . . . . ?
C4 C5 N1 C1 0.7(11) . . . . ?
C4 C5 N1 Pd1 -178.7(6) . . . . ?
C2 C1 N1 C5 -0.3(11) . . . . ?
C2 C1 N1 Pd1 179.1(6) . . . . ?
N3 C6 N2 C8 -1.1(7) . . . . ?
Pd1 C6 N2 C8 172.6(5) . . . . ?
N3 C6 N2 C9 175.4(5) . . . . ?
Pd1 C6 N2 C9 -11.0(9) . . . . ?
C7 C8 N2 C6 0.9(7) . . . . ?
C7 C8 N2 C9 -175.6(6) . . . . ?
C14 C9 N2 C6 -42.0(9) . . . . ?
C10 C9 N2 C6 137.8(6) . . . . ?
C14 C9 N2 C8 133.9(7) . . . . ?
C10 C9 N2 C8 -46.3(9) . . . . ?
N2 C6 N3 C7 0.9(7) . . . . ?
Pd1 C6 N3 C7 -172.9(5) . . . . ?
N2 C6 N3 C19 -175.3(6) . . . . ?
Pd1 C6 N3 C19 10.9(9) . . . . ?
C8 C7 N3 C6 -0.4(8) . . . . ?
C8 C7 N3 C19 175.8(7) . . . . ?
C20 C19 N3 C6 -73.7(9) . . . . ?
C20 C19 N3 C7 110.7(9) . . . . ?
C15 C16 N4 N5 -1.1(8) . . . . ?
Au1 C16 N4 N5 -179.9(5) . . . . ?
C15 C16 N4 C12 177.4(6) . . . . ?
Au1 C16 N4 C12 -1.4(10) . . . . ?
C11 C12 N4 N5 35.6(9) . . . . ?
C13 C12 N4 N5 -144.8(6) . . . . ?
C11 C12 N4 C16 -142.8(7) . . . . ?
C13 C12 N4 C16 36.8(10) . . . . ?
C16 N4 N5 N6 0.7(8) . . . . ?
C12 N4 N5 N6 -178.0(6) . . . . ?
N4 N5 N6 C15 0.1(8) . . . . ?
N4 N5 N6 C17 179.0(7) . . . . ?
C16 C15 N6 N5 -0.8(9) . . . . ?
C16 C15 N6 C17 -179.6(8) . . . . ?
C18 C17 N6 N5 58.1(12) . . . . ?
C18 C17 N6 C15 -123.1(11) . . . . ?

_refine_diff_density_max         1.100
_refine_diff_density_min         -1.966
_refine_diff_density_rms         0.164



####################################################################### 
# 
# 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_shelx_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 2176105'
loop_
_audit_author_name
_audit_author_address
'Arnab Rit'
;IIT Madras
India
;
_audit_update_record             
;
2022-05-31 deposited with the CCDC.	2022-10-21 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         'C30 H36 Br3 Ir N6 Pd'
_chemical_formula_sum            'C30 H36 Br3 Ir N6 Pd'
_chemical_formula_weight         1018.98

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

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

_cell_length_a                   25.915(2)
_cell_length_b                   20.090(2)
_cell_length_c                   15.4825(16)
_cell_angle_alpha                90
_cell_angle_beta                 115.662(5)
_cell_angle_gamma                90
_cell_volume                     7265.5(13)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)

_cell_measurement_reflns_used    9059
_cell_measurement_theta_min      3.11
_cell_measurement_theta_max      25.68
_exptl_crystal_description       BLOCK
_exptl_crystal_colour            brown


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.863
_exptl_crystal_F_000             3888
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    7.481
_shelx_estimated_absorpt_T_min   0.316
_shelx_estimated_absorpt_T_max   0.522
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4862
_exptl_absorpt_correction_T_max  0.6463
_exptl_absorpt_process_details   'SADABS (Bruker, 2016)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a

_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  
'Bruker D8 VENTURE diffractometer with PHOTON 100 CMOS detector'
_diffrn_measurement_method       'ω and φ scan'

_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            52952
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_av_R_equivalents  0.0648
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.165
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             6379
_reflns_number_gt                4464
_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.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'APEX3 (Bruker, 2016)'
_computing_cell_refinement       'APEX3/SAINT (Bruker, 2016)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2016)'

_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    
'ORTEP3 (Farrugia, 1997) and Mercury (Bruno et al., 2002)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'


_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)+(0.0304P)²+162.0853P] 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         6379
_refine_ls_number_parameters     450
_refine_ls_number_restraints     462
_refine_ls_R_factor_all          0.0974
_refine_ls_R_factor_gt           0.0571
_refine_ls_wR_factor_ref         0.1504
_refine_ls_wR_factor_gt          0.1172
_refine_ls_goodness_of_fit_ref   1.211
_refine_ls_restrained_S_all      1.183
_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
Pd1 Pd 0.59925(4) 0.32835(5) 0.33477(7) 0.0635(3) Uani 1 1 d . U . . .
Ir1 Ir 0.36156(2) 0.11146(3) 0.51591(4) 0.06271(18) Uani 1 1 d . U . . .
C1 C 0.3529(8) 0.2208(7) 0.5260(13) 0.090(3) Uani 1 1 d . U . . .
C2 C 0.3643(7) 0.1902(7) 0.6127(11) 0.080(3) Uani 1 1 d . U . . .
C3 C 0.3167(6) 0.1475(7) 0.6013(12) 0.079(3) Uani 1 1 d . U . . .
C4 C 0.2772(6) 0.1515(9) 0.5036(13) 0.093(4) Uani 1 1 d . U . . .
C5 C 0.3019(8) 0.1979(8) 0.4598(12) 0.091(3) Uani 1 1 d . U . . .
C6 C 0.2190(7) 0.1182(12) 0.4548(18) 0.154(9) Uani 1 1 d . U . . .
H6A H 0.207546 0.116040 0.387019 0.231 Uiso 1 1 calc R U . . .
H6B H 0.191388 0.143537 0.466877 0.231 Uiso 1 1 calc R U . . .
H6C H 0.221231 0.073974 0.479684 0.231 Uiso 1 1 calc R U . . .
C7 C 0.3114(9) 0.1120(9) 0.6801(14) 0.121(6) Uani 1 1 d . U . . .
H7A H 0.318303 0.142366 0.731777 0.182 Uiso 1 1 calc R U . . .
H7B H 0.338936 0.076545 0.702137 0.182 Uiso 1 1 calc R U . . .
H7C H 0.273528 0.093863 0.657751 0.182 Uiso 1 1 calc R U . . .
C8 C 0.4124(9) 0.1993(10) 0.7093(14) 0.131(7) Uani 1 1 d . U . . .
H8A H 0.421005 0.157504 0.742672 0.196 Uiso 1 1 calc R U . . .
H8B H 0.401724 0.231219 0.744736 0.196 Uiso 1 1 calc R U . . .
H8C H 0.445521 0.214934 0.702728 0.196 Uiso 1 1 calc R U . . .
C9 C 0.3906(11) 0.2733(8) 0.5141(19) 0.160(9) Uani 1 1 d . U . . .
H9A H 0.429689 0.265159 0.558328 0.239 Uiso 1 1 calc R U . . .
H9B H 0.379145 0.316360 0.526533 0.239 Uiso 1 1 calc R U . . .
H9C H 0.387049 0.272081 0.449746 0.239 Uiso 1 1 calc R U . . .
C10 C 0.2741(11) 0.2195(12) 0.3594(13) 0.178(11) Uani 1 1 d . U . . .
H10A H 0.245227 0.187802 0.322441 0.267 Uiso 1 1 calc R U . . .
H10B H 0.302138 0.222508 0.334510 0.267 Uiso 1 1 calc R U . . .
H10C H 0.256761 0.262284 0.355483 0.267 Uiso 1 1 calc R U . . .
C20 C 0.5445(5) 0.2302(6) 0.4211(8) 0.057(2) Uani 1 1 d . U . . .
H20 H 0.507860 0.229023 0.371000 0.068 Uiso 1 1 calc R U . . .
C21 C 0.5889(6) 0.2680(7) 0.4247(9) 0.069(3) Uani 1 1 d . U . . .
N3 N 0.5627(4) 0.1954(5) 0.5016(7) 0.060(2) Uani 1 1 d . U . . .
N4 N 0.6164(5) 0.2079(6) 0.5594(8) 0.078(3) Uani 1 1 d . U . . .
N5 N 0.6308(4) 0.2535(6) 0.5105(8) 0.073(3) Uani 1 1 d . U . . .
C22 C 0.6920(7) 0.2777(10) 0.5588(14) 0.120(7) Uani 1 1 d . U . . .
H22A H 0.717198 0.242005 0.595174 0.144 Uiso 1 1 calc R U . . .
H22B H 0.704262 0.293314 0.511376 0.144 Uiso 1 1 calc R U . . .
C23 C 0.6934(14) 0.3304(18) 0.620(2) 0.254(19) Uani 1 1 d . U . . .
H23A H 0.731521 0.335222 0.670161 0.381 Uiso 1 1 calc R U . . .
H23B H 0.667625 0.320705 0.648424 0.381 Uiso 1 1 calc R U . . .
H23C H 0.681847 0.371011 0.584363 0.381 Uiso 1 1 calc R U . . .
Br3 Br 0.32921(7) 0.05587(8) 0.35625(12) 0.0881(5) Uani 1 1 d . U . . .
N1 N 0.3640(5) -0.0296(5) 0.5959(9) 0.079(3) Uani 1 1 d D U . . .
N2 N 0.4441(4) 0.0073(4) 0.6038(7) 0.059(2) Uani 1 1 d D U . . .
C11 C 0.3878(5) 0.0245(6) 0.5741(10) 0.066(2) Uani 1 1 d D U . . .
C12 C 0.4050(5) -0.0778(6) 0.6368(11) 0.078(3) Uani 1 1 d D U . . .
H12 H 0.399247 -0.119135 0.658365 0.094 Uiso 1 1 calc R U . . .
C13 C 0.4550(6) -0.0555(5) 0.6407(9) 0.068(3) Uani 1 1 d D U . . .
H13 H 0.489724 -0.078145 0.663683 0.082 Uiso 1 1 calc R U . . .
C14 C 0.4775(4) 0.0535(5) 0.5824(7) 0.051(2) Uani 1 1 d D U . . .
C15 C 0.4453(4) 0.1088(5) 0.5329(7) 0.053(2) Uani 1 1 d D U . . .
C16 C 0.4748(4) 0.1552(5) 0.5048(8) 0.055(2) Uani 1 1 d D U . . .
H16 H 0.456112 0.192839 0.470713 0.066 Uiso 1 1 calc R U . . .
C17 C 0.5323(4) 0.1453(6) 0.5277(8) 0.056(2) Uani 1 1 d D U . . .
C18 C 0.5635(5) 0.0916(5) 0.5786(8) 0.061(3) Uani 1 1 d D U . . .
H18 H 0.602354 0.087749 0.594377 0.073 Uiso 1 1 calc R U . . .
C19 C 0.5352(5) 0.0437(6) 0.6053(9) 0.060(2) Uani 1 1 d D U . . .
H19 H 0.554196 0.005740 0.637965 0.072 Uiso 1 1 calc R U . . .
C24 C 0.3035(6) -0.0387(8) 0.5731(15) 0.121(7) Uani 1 1 d D U . . .
H24A H 0.282763 0.002328 0.547736 0.145 Uiso 1 1 calc R U . . .
H24B H 0.299487 -0.050193 0.630755 0.145 Uiso 1 1 calc R U . . .
C25 C 0.2793(10) -0.0927(12) 0.5012(18) 0.182(11) Uani 1 1 d D U . . .
H25A H 0.238512 -0.093939 0.478448 0.273 Uiso 1 1 calc R U . . .
H25B H 0.295331 -0.134650 0.530269 0.273 Uiso 1 1 calc R U . . .
H25C H 0.288581 -0.084540 0.448430 0.273 Uiso 1 1 calc R U . . .
N6 N 0.6102(14) 0.3904(19) 0.235(3) 0.085(6) Uani 0.53(3) 1 d D U P A 1
C26 C 0.5590(18) 0.4003(17) 0.156(2) 0.113(9) Uani 0.53(3) 1 d D U P A 1
H26 H 0.525059 0.380494 0.149777 0.135 Uiso 0.53(3) 1 calc R U P A 1
C27 C 0.562(2) 0.4422(17) 0.087(3) 0.128(10) Uani 0.53(3) 1 d D U P A 1
H27 H 0.528944 0.453243 0.032338 0.154 Uiso 0.53(3) 1 calc R U P A 1
C28 C 0.6149(19) 0.467(2) 0.102(3) 0.129(10) Uani 0.53(3) 1 d D U P A 1
H28 H 0.617265 0.490831 0.052031 0.155 Uiso 0.53(3) 1 calc R U P A 1
C29 C 0.6643(19) 0.459(2) 0.185(3) 0.113(9) Uani 0.53(3) 1 d D U P A 1
H29 H 0.697776 0.481663 0.193832 0.136 Uiso 0.53(3) 1 calc R U P A 1
C30 C 0.6627(16) 0.4172(18) 0.255(3) 0.101(8) Uani 0.53(3) 1 d D U P A 1
H30 H 0.694977 0.407930 0.311709 0.121 Uiso 0.53(3) 1 calc R U P A 1
Br1 Br 0.6099(4) 0.2351(5) 0.2501(6) 0.0759(19) Uani 0.53(3) 1 d . U P A 1
Br2 Br 0.5946(7) 0.4193(7) 0.4229(11) 0.130(4) Uani 0.53(3) 1 d . U P A 1
N6' N 0.6129(15) 0.392(2) 0.242(2) 0.078(6) Uani 0.47(3) 1 d D U P A 2
C26' C 0.5820(14) 0.3946(16) 0.146(2) 0.078(7) Uani 0.47(3) 1 d D U P A 2
H26' H 0.550006 0.367301 0.116946 0.094 Uiso 0.47(3) 1 calc R U P A 2
C27' C 0.5964(15) 0.4359(15) 0.088(2) 0.088(8) Uani 0.47(3) 1 d D U P A 2
H27' H 0.574193 0.436151 0.022536 0.106 Uiso 0.47(3) 1 calc R U P A 2
C28' C 0.6437(15) 0.4771(19) 0.129(2) 0.094(8) Uani 0.47(3) 1 d D U P A 2
H28' H 0.653081 0.506451 0.091212 0.113 Uiso 0.47(3) 1 calc R U P A 2
C29' C 0.6767(17) 0.473(2) 0.227(2) 0.100(9) Uani 0.47(3) 1 d D U P A 2
H29' H 0.711853 0.494205 0.255451 0.119 Uiso 0.47(3) 1 calc R U P A 2
C30' C 0.6577(16) 0.4367(18) 0.284(3) 0.090(8) Uani 0.47(3) 1 d D U P A 2
H30' H 0.675007 0.442431 0.350159 0.109 Uiso 0.47(3) 1 calc R U P A 2
Br1' Br 0.6292(12) 0.2340(7) 0.2724(16) 0.143(4) Uani 0.47(3) 1 d . U P A 2
Br2' Br 0.5691(12) 0.4205(8) 0.4029(14) 0.156(6) Uani 0.47(3) 1 d . U P A 2


_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
Pd1 C21 1.950(12) . ?
Pd1 N6' 2.06(4) . ?
Pd1 N6 2.09(4) . ?
Pd1 Br2 2.315(11) . ?
Pd1 Br1 2.371(9) . ?
Pd1 Br1' 2.403(13) . ?
Pd1 Br2' 2.422(14) . ?
Ir1 C11 1.948(11) . ?
Ir1 C15 2.070(10) . ?
Ir1 C2 2.160(13) . ?
Ir1 C1 2.220(14) . ?
Ir1 C3 2.226(13) . ?
Ir1 C5 2.234(13) . ?
Ir1 C4 2.257(13) . ?
Ir1 Br3 2.5032(17) . ?
C1 C5 1.35(2) . ?
C1 C2 1.39(2) . ?
C1 C9 1.50(2) . ?
C2 C3 1.45(2) . ?
C2 C8 1.49(2) . ?
C3 C4 1.41(2) . ?
C3 C7 1.47(2) . ?
C4 C5 1.45(2) . ?
C4 C6 1.52(2) . ?
C5 C10 1.47(2) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C20 N3 1.327(14) . ?
C20 C21 1.360(16) . ?
C20 H20 0.9300 . ?
C21 N5 1.334(16) . ?
N3 N4 1.312(13) . ?
N3 C17 1.439(14) . ?
N4 N5 1.340(13) . ?
N5 C22 1.510(17) . ?
C22 C23 1.41(3) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
N1 C11 1.362(12) . ?
N1 C12 1.374(13) . ?
N1 C24 1.462(13) . ?
N2 C13 1.363(12) . ?
N2 C11 1.371(12) . ?
N2 C14 1.402(13) . ?
C12 C13 1.349(13) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 C19 1.394(12) . ?
C14 C15 1.401(12) . ?
C15 C16 1.391(12) . ?
C16 C17 1.387(12) . ?
C16 H16 0.9300 . ?
C17 C18 1.373(13) . ?
C18 C19 1.378(12) . ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?
C24 C25 1.484(17) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
N6 C30 1.369(19) . ?
N6 C26 1.374(19) . ?
C26 C27 1.390(19) . ?
C26 H26 0.9300 . ?
C27 C28 1.389(19) . ?
C27 H27 0.9300 . ?
C28 C29 1.375(19) . ?
C28 H28 0.9300 . ?
C29 C30 1.397(19) . ?
C29 H29 0.9300 . ?
C30 H30 0.9300 . ?
N6' C26' 1.361(19) . ?
N6' C30' 1.384(19) . ?
C26' C27' 1.378(19) . ?
C26' H26' 0.9300 . ?
C27' C28' 1.382(19) . ?
C27' H27' 0.9300 . ?
C28' C29' 1.395(19) . ?
C28' H28' 0.9300 . ?
C29' C30' 1.380(19) . ?
C29' H29' 0.9300 . ?
C30' H30' 0.9300 . ?

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
C21 Pd1 N6' 178.2(10) . . ?
C21 Pd1 N6 178.1(10) . . ?
C21 Pd1 Br2 90.7(6) . . ?
N6 Pd1 Br2 91.3(10) . . ?
C21 Pd1 Br1 89.4(5) . . ?
N6 Pd1 Br1 88.7(10) . . ?
Br2 Pd1 Br1 176.6(4) . . ?
C21 Pd1 Br1' 88.0(5) . . ?
N6' Pd1 Br1' 91.7(12) . . ?
C21 Pd1 Br2' 89.7(6) . . ?
N6' Pd1 Br2' 90.6(12) . . ?
Br1' Pd1 Br2' 177.6(5) . . ?
C11 Ir1 C15 77.3(4) . . ?
C11 Ir1 C2 115.9(6) . . ?
C15 Ir1 C2 102.3(5) . . ?
C11 Ir1 C1 151.7(6) . . ?
C15 Ir1 C1 98.6(5) . . ?
C2 Ir1 C1 36.9(6) . . ?
C11 Ir1 C3 100.6(5) . . ?
C15 Ir1 C3 136.2(5) . . ?
C2 Ir1 C3 38.6(5) . . ?
C1 Ir1 C3 62.7(5) . . ?
C11 Ir1 C5 157.0(6) . . ?
C15 Ir1 C5 125.4(6) . . ?
C2 Ir1 C5 60.7(6) . . ?
C1 Ir1 C5 35.4(6) . . ?
C3 Ir1 C5 61.8(5) . . ?
C11 Ir1 C4 119.3(6) . . ?
C15 Ir1 C4 160.6(5) . . ?
C2 Ir1 C4 62.4(6) . . ?
C1 Ir1 C4 61.9(6) . . ?
C3 Ir1 C4 36.8(5) . . ?
C5 Ir1 C4 37.8(6) . . ?
C11 Ir1 Br3 87.5(4) . . ?
C15 Ir1 Br3 89.9(3) . . ?
C2 Ir1 Br3 155.3(4) . . ?
C1 Ir1 Br3 120.7(5) . . ?
C3 Ir1 Br3 133.9(4) . . ?
C5 Ir1 Br3 94.8(4) . . ?
C4 Ir1 Br3 100.2(4) . . ?
C5 C1 C2 108.2(15) . . ?
C5 C1 C9 128.2(19) . . ?
C2 C1 C9 123(2) . . ?
C5 C1 Ir1 72.9(9) . . ?
C2 C1 Ir1 69.2(8) . . ?
C9 C1 Ir1 126.5(10) . . ?
C1 C2 C3 109.2(15) . . ?
C1 C2 C8 130.9(17) . . ?
C3 C2 C8 119.7(15) . . ?
C1 C2 Ir1 73.9(8) . . ?
C3 C2 Ir1 73.2(8) . . ?
C8 C2 Ir1 123.3(12) . . ?
C4 C3 C2 106.3(14) . . ?
C4 C3 C7 129.2(16) . . ?
C2 C3 C7 124.4(16) . . ?
C4 C3 Ir1 72.9(8) . . ?
C2 C3 Ir1 68.3(7) . . ?
C7 C3 Ir1 126.6(10) . . ?
C3 C4 C5 106.0(15) . . ?
C3 C4 C6 127.5(18) . . ?
C5 C4 C6 126.4(18) . . ?
C3 C4 Ir1 70.4(8) . . ?
C5 C4 Ir1 70.2(7) . . ?
C6 C4 Ir1 127.0(11) . . ?
C1 C5 C4 110.3(14) . . ?
C1 C5 C10 125(2) . . ?
C4 C5 C10 125(2) . . ?
C1 C5 Ir1 71.7(9) . . ?
C4 C5 Ir1 72.0(8) . . ?
C10 C5 Ir1 125.6(10) . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C3 C7 H7A 109.5 . . ?
C3 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C3 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C2 C8 H8A 109.5 . . ?
C2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C1 C9 H9A 109.5 . . ?
C1 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C1 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C5 C10 H10A 109.5 . . ?
C5 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C5 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N3 C20 C21 107.8(11) . . ?
N3 C20 H20 126.1 . . ?
C21 C20 H20 126.1 . . ?
N5 C21 C20 103.2(11) . . ?
N5 C21 Pd1 122.9(9) . . ?
C20 C21 Pd1 133.9(10) . . ?
N4 N3 C20 112.3(10) . . ?
N4 N3 C17 119.4(10) . . ?
C20 N3 C17 128.2(10) . . ?
N3 N4 N5 102.7(10) . . ?
C21 N5 N4 113.9(10) . . ?
C21 N5 C22 130.5(12) . . ?
N4 N5 C22 115.5(11) . . ?
C23 C22 N5 107(2) . . ?
C23 C22 H22A 110.3 . . ?
N5 C22 H22A 110.3 . . ?
C23 C22 H22B 110.3 . . ?
N5 C22 H22B 110.3 . . ?
H22A C22 H22B 108.6 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C11 N1 C12 109.5(10) . . ?
C11 N1 C24 126.5(12) . . ?
C12 N1 C24 123.9(11) . . ?
C13 N2 C11 111.8(10) . . ?
C13 N2 C14 132.4(9) . . ?
C11 N2 C14 115.5(9) . . ?
N1 C11 N2 104.3(10) . . ?
N1 C11 Ir1 136.5(9) . . ?
N2 C11 Ir1 119.3(8) . . ?
C13 C12 N1 108.8(11) . . ?
C13 C12 H12 125.6 . . ?
N1 C12 H12 125.6 . . ?
C12 C13 N2 105.6(11) . . ?
C12 C13 H13 127.2 . . ?
N2 C13 H13 127.2 . . ?
C19 C14 C15 124.7(10) . . ?
C19 C14 N2 123.4(9) . . ?
C15 C14 N2 111.8(9) . . ?
C16 C15 C14 115.1(9) . . ?
C16 C15 Ir1 129.2(8) . . ?
C14 C15 Ir1 115.7(7) . . ?
C17 C16 C15 120.0(10) . . ?
C17 C16 H16 120.0 . . ?
C15 C16 H16 120.0 . . ?
C18 C17 C16 124.1(10) . . ?
C18 C17 N3 116.8(9) . . ?
C16 C17 N3 119.0(10) . . ?
C17 C18 C19 117.5(10) . . ?
C17 C18 H18 121.3 . . ?
C19 C18 H18 121.3 . . ?
C18 C19 C14 118.6(11) . . ?
C18 C19 H19 120.7 . . ?
C14 C19 H19 120.7 . . ?
N1 C24 C25 109.4(15) . . ?
N1 C24 H24A 109.8 . . ?
C25 C24 H24A 109.8 . . ?
N1 C24 H24B 109.8 . . ?
C25 C24 H24B 109.8 . . ?
H24A C24 H24B 108.2 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C30 N6 C26 129(4) . . ?
C30 N6 Pd1 120(3) . . ?
C26 N6 Pd1 111(2) . . ?
N6 C26 C27 115(4) . . ?
N6 C26 H26 122.5 . . ?
C27 C26 H26 122.5 . . ?
C28 C27 C26 118(4) . . ?
C28 C27 H27 121.0 . . ?
C26 C27 H27 121.0 . . ?
C29 C28 C27 125(4) . . ?
C29 C28 H28 117.6 . . ?
C27 C28 H28 117.6 . . ?
C28 C29 C30 118(4) . . ?
C28 C29 H29 121.1 . . ?
C30 C29 H29 121.1 . . ?
N6 C30 C29 115(4) . . ?
N6 C30 H30 122.4 . . ?
C29 C30 H30 122.4 . . ?
C26' N6' C30' 118(4) . . ?
C26' N6' Pd1 126(3) . . ?
C30' N6' Pd1 116(2) . . ?
N6' C26' C27' 122(3) . . ?
N6' C26' H26' 118.8 . . ?
C27' C26' H26' 118.8 . . ?
C26' C27' C28' 120(3) . . ?
C26' C27' H27' 119.8 . . ?
C28' C27' H27' 119.8 . . ?
C27' C28' C29' 117(3) . . ?
C27' C28' H28' 121.4 . . ?
C29' C28' H28' 121.4 . . ?
C30' C29' C28' 121(3) . . ?
C30' C29' H29' 119.6 . . ?
C28' C29' H29' 119.6 . . ?
C29' C30' N6' 120(4) . . ?
C29' C30' H30' 120.0 . . ?
N6' C30' H30' 120.0 . . ?

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
C5 C1 C2 C3 -2.3(16) . . . . ?
C9 C1 C2 C3 174.1(13) . . . . ?
Ir1 C1 C2 C3 -65.2(9) . . . . ?
C5 C1 C2 C8 -176.7(16) . . . . ?
C9 C1 C2 C8 0(2) . . . . ?
Ir1 C1 C2 C8 120.4(17) . . . . ?
C5 C1 C2 Ir1 62.9(10) . . . . ?
C9 C1 C2 Ir1 -120.8(14) . . . . ?
C1 C2 C3 C4 2.2(15) . . . . ?
C8 C2 C3 C4 177.4(14) . . . . ?
Ir1 C2 C3 C4 -63.4(10) . . . . ?
C1 C2 C3 C7 -174.1(13) . . . . ?
C8 C2 C3 C7 1(2) . . . . ?
Ir1 C2 C3 C7 120.3(14) . . . . ?
C1 C2 C3 Ir1 65.6(9) . . . . ?
C8 C2 C3 Ir1 -119.2(14) . . . . ?
C2 C3 C4 C5 -1.2(15) . . . . ?
C7 C3 C4 C5 174.8(14) . . . . ?
Ir1 C3 C4 C5 -61.6(9) . . . . ?
C2 C3 C4 C6 -177.4(14) . . . . ?
C7 C3 C4 C6 -1(3) . . . . ?
Ir1 C3 C4 C6 122.2(16) . . . . ?
C2 C3 C4 Ir1 60.4(9) . . . . ?
C7 C3 C4 Ir1 -123.5(16) . . . . ?
C2 C1 C5 C4 1.5(16) . . . . ?
C9 C1 C5 C4 -174.6(14) . . . . ?
Ir1 C1 C5 C4 62.0(10) . . . . ?
C2 C1 C5 C10 178.4(13) . . . . ?
C9 C1 C5 C10 2(2) . . . . ?
Ir1 C1 C5 C10 -121.1(14) . . . . ?
C2 C1 C5 Ir1 -60.5(10) . . . . ?
C9 C1 C5 Ir1 123.3(15) . . . . ?
C3 C4 C5 C1 -0.1(16) . . . . ?
C6 C4 C5 C1 176.1(14) . . . . ?
Ir1 C4 C5 C1 -61.9(10) . . . . ?
C3 C4 C5 C10 -177.0(14) . . . . ?
C6 C4 C5 C10 -1(2) . . . . ?
Ir1 C4 C5 C10 121.2(14) . . . . ?
C3 C4 C5 Ir1 61.7(9) . . . . ?
C6 C4 C5 Ir1 -122.0(15) . . . . ?
N3 C20 C21 N5 -1.4(14) . . . . ?
N3 C20 C21 Pd1 176.2(11) . . . . ?
C21 C20 N3 N4 0.6(15) . . . . ?
C21 C20 N3 C17 -175.5(11) . . . . ?
C20 N3 N4 N5 0.5(14) . . . . ?
C17 N3 N4 N5 177.0(10) . . . . ?
C20 C21 N5 N4 1.9(16) . . . . ?
Pd1 C21 N5 N4 -176.1(10) . . . . ?
C20 C21 N5 C22 179.0(16) . . . . ?
Pd1 C21 N5 C22 1(2) . . . . ?
N3 N4 N5 C21 -1.5(16) . . . . ?
N3 N4 N5 C22 -179.1(13) . . . . ?
C21 N5 C22 C23 97(2) . . . . ?
N4 N5 C22 C23 -86(2) . . . . ?
C12 N1 C11 N2 -0.5(15) . . . . ?
C24 N1 C11 N2 -175.7(14) . . . . ?
C12 N1 C11 Ir1 179.5(12) . . . . ?
C24 N1 C11 Ir1 4(2) . . . . ?
C13 N2 C11 N1 1.4(15) . . . . ?
C14 N2 C11 N1 175.3(10) . . . . ?
C13 N2 C11 Ir1 -178.6(9) . . . . ?
C14 N2 C11 Ir1 -4.7(14) . . . . ?
C11 N1 C12 C13 -0.6(17) . . . . ?
C24 N1 C12 C13 174.8(15) . . . . ?
N1 C12 C13 N2 1.4(16) . . . . ?
C11 N2 C13 C12 -1.8(15) . . . . ?
C14 N2 C13 C12 -174.3(12) . . . . ?
C13 N2 C14 C19 -6.3(19) . . . . ?
C11 N2 C14 C19 -178.6(11) . . . . ?
C13 N2 C14 C15 171.7(12) . . . . ?
C11 N2 C14 C15 -0.6(13) . . . . ?
C19 C14 C15 C16 1.1(12) . . . . ?
N2 C14 C15 C16 -176.9(9) . . . . ?
C19 C14 C15 Ir1 -176.8(9) . . . . ?
N2 C14 C15 Ir1 5.1(10) . . . . ?
C14 C15 C16 C17 -1.0(12) . . . . ?
Ir1 C15 C16 C17 176.6(8) . . . . ?
C15 C16 C17 C18 -0.7(17) . . . . ?
C15 C16 C17 N3 -177.3(9) . . . . ?
N4 N3 C17 C18 -33.3(16) . . . . ?
C20 N3 C17 C18 142.4(12) . . . . ?
N4 N3 C17 C16 143.5(12) . . . . ?
C20 N3 C17 C16 -40.7(17) . . . . ?
C16 C17 C18 C19 2.4(18) . . . . ?
N3 C17 C18 C19 179.0(10) . . . . ?
C17 C18 C19 C14 -2.2(17) . . . . ?
C15 C14 C19 C18 0.5(16) . . . . ?
N2 C14 C19 C18 178.3(10) . . . . ?
C11 N1 C24 C25 112.3(19) . . . . ?
C12 N1 C24 C25 -62(2) . . . . ?
C30 N6 C26 C27 2(2) . . . . ?
Pd1 N6 C26 C27 179(2) . . . . ?
N6 C26 C27 C28 3(2) . . . . ?
C26 C27 C28 C29 -7(5) . . . . ?
C27 C28 C29 C30 8(6) . . . . ?
C26 N6 C30 C29 -1(4) . . . . ?
Pd1 N6 C30 C29 -178(3) . . . . ?
C28 C29 C30 N6 -3(5) . . . . ?
C30' N6' C26' C27' 5(2) . . . . ?
Pd1 N6' C26' C27' -176(3) . . . . ?
N6' C26' C27' C28' 0(2) . . . . ?
C26' C27' C28' C29' 2(4) . . . . ?
C27' C28' C29' C30' -10(5) . . . . ?
C28' C29' C30' N6' 15(6) . . . . ?
C26' N6' C30' C29' -12(4) . . . . ?
Pd1 N6' C30' C29' 168(3) . . . . ?

_refine_diff_density_max         1.270
_refine_diff_density_min         -0.925
_refine_diff_density_rms         0.152




# start Validation Reply Form
_vrf_PLAT342_shelx               
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.02385 Ang.  
RESPONSE: The crystal lattice contains disordered moieties. Hence
accuracies in bond lengths are low
;
_vrf_PLAT910_shelx               
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         14 Note  
RESPONSE: These reflections are affected by the beam stop. Hence omitted 
fromrefinement
;
# end Validation Reply Form



####################################################################### 
# 
# 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_PR15
_database_code_depnum_ccdc_archive 'CCDC 2176101'
loop_
_audit_author_name
_audit_author_address
'Arnab Rit'
;IIT Madras
India
;
_audit_update_record             
;
2022-05-31 deposited with the CCDC.	2022-10-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C25 H32 I Ir N5), 2(I), H2 O'

_chemical_formula_sum            'C50 H66 I4 Ir2 N10 O'
_chemical_formula_weight         1715.12

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ir Ir -4.7710 6.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.1579(3)
_cell_length_b                   12.7784(3)
_cell_length_c                   22.2614(5)
_cell_angle_alpha                95.693(2)
_cell_angle_beta                 98.9580(10)
_cell_angle_gamma                94.414(2)
_cell_volume                     2827.66(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    9916
_cell_measurement_theta_min      3.49
_cell_measurement_theta_max      66.84

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.014
_exptl_crystal_F_000             1620
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    26.465
_shelx_estimated_absorpt_T_min   0.109
_shelx_estimated_absorpt_T_max   0.177
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3397
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_process_details   'SADABS (Bruker, 2016)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a

_diffrn_radiation_source         'micro-focus sealed tube'
_diffrn_measurement_device_type  'Bruker axs kappa apex3 CMOS Diffractometer'
_diffrn_measurement_method       'ω and φ scan'



_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            70001
_diffrn_reflns_av_unetI/netI     0.0599
_diffrn_reflns_av_R_equivalents  0.1045
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.491
_diffrn_reflns_theta_max         66.957
_diffrn_reflns_theta_full        66.957
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             10047
_reflns_number_gt                7056
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'APEX3(Bruker, 2016)'
_computing_cell_refinement       'APEX3/SAINT (Bruker, 2016)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2016)'
_computing_structure_solution    'SHELXT-2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    
'ORTEP3 (Farrugia, 1997) and Mercury (Bruno et al., 2002)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'



_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0484P)²+52.0581P] 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     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10047
_refine_ls_number_parameters     629
_refine_ls_number_restraints     110
_refine_ls_R_factor_all          0.0888
_refine_ls_R_factor_gt           0.0581
_refine_ls_wR_factor_ref         0.1456
_refine_ls_wR_factor_gt          0.1310
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.027
_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
C1 C 0.3681(11) 0.8537(9) 0.7866(5) 0.027(3) Uani 1 1 d . . . . .
C2 C 0.4181(13) 0.7898(11) 0.8312(6) 0.040(3) Uani 1 1 d . . . . .
C3 C 0.3804(14) 0.8315(13) 0.8884(6) 0.048(4) Uani 1 1 d . . . . .
C4 C 0.3112(13) 0.9193(12) 0.8786(6) 0.046(4) Uani 1 1 d . . . . .
C5 C 0.2970(13) 0.9319(10) 0.8144(7) 0.043(3) Uani 1 1 d . . . . .
C6 C 0.2423(17) 1.0238(13) 0.7854(10) 0.085(7) Uani 1 1 d . . . . .
H6A H 0.1989 1.0644 0.8139 0.127 Uiso 1 1 calc R U . . .
H6B H 0.3141 1.0675 0.7745 0.127 Uiso 1 1 calc R U . . .
H6C H 0.1788 0.9985 0.7493 0.127 Uiso 1 1 calc R U . . .
C7 C 0.2780(19) 0.9976(16) 0.9273(9) 0.103(8) Uani 1 1 d . . . . .
H7A H 0.2297 1.0509 0.9086 0.155 Uiso 1 1 calc R U . . .
H7B H 0.2238 0.9621 0.9522 0.155 Uiso 1 1 calc R U . . .
H7C H 0.3592 1.0300 0.9524 0.155 Uiso 1 1 calc R U . . .
C8 C 0.4203(19) 0.7915(19) 0.9485(7) 0.101(8) Uani 1 1 d . . . . .
H8A H 0.4670 0.7297 0.9428 0.152 Uiso 1 1 calc R U . . .
H8B H 0.4778 0.8452 0.9756 0.152 Uiso 1 1 calc R U . . .
H8C H 0.3418 0.7739 0.9659 0.152 Uiso 1 1 calc R U . . .
C9 C 0.4996(14) 0.6995(13) 0.8250(10) 0.078(6) Uani 1 1 d . . . . .
H9A H 0.5182 0.6718 0.8637 0.116 Uiso 1 1 calc R U . . .
H9B H 0.4512 0.6454 0.7949 0.116 Uiso 1 1 calc R U . . .
H9C H 0.5822 0.7227 0.8125 0.116 Uiso 1 1 calc R U . . .
C10 C 0.3996(16) 0.8491(14) 0.7226(6) 0.062(5) Uani 1 1 d . . . . .
H10A H 0.3532 0.9006 0.7012 0.093 Uiso 1 1 calc R U . . .
H10B H 0.4943 0.8639 0.7243 0.093 Uiso 1 1 calc R U . . .
H10C H 0.3713 0.7799 0.7015 0.093 Uiso 1 1 calc R U . . .
C11 C -0.0002(12) 0.8045(9) 0.7989(5) 0.032(3) Uani 1 1 d . . . . .
C12 C -0.2106(14) 0.8539(11) 0.7863(6) 0.046(3) Uani 1 1 d . . . . .
H12 H -0.2858 0.8872 0.7934 0.055 Uiso 1 1 calc R U . . .
C13 C -0.2002(13) 0.7882(12) 0.7369(6) 0.045(3) Uani 1 1 d . . . . .
H13 H -0.2672 0.7675 0.7034 0.054 Uiso 1 1 calc R U . . .
C14 C -0.0068(11) 0.6872(9) 0.7100(5) 0.028(3) Uani 1 1 d . . . . .
C15 C 0.1283(12) 0.6832(9) 0.7364(5) 0.029(3) Uani 1 1 d . . . . .
C16 C 0.1998(13) 0.6163(9) 0.7046(5) 0.035(3) Uani 1 1 d . . . . .
H16 H 0.2884 0.6087 0.7205 0.042 Uiso 1 1 calc R U . . .
C17 C 0.1417(14) 0.5604(10) 0.6496(6) 0.038(3) Uani 1 1 d . . . . .
C18 C 0.0076(14) 0.5628(11) 0.6247(6) 0.046(4) Uani 1 1 d . . . . .
H18 H -0.0302 0.5224 0.5882 0.056 Uiso 1 1 calc R U . . .
C19 C -0.0670(14) 0.6277(11) 0.6565(5) 0.041(3) Uani 1 1 d . . . . .
H19 H -0.1572 0.6312 0.6417 0.049 Uiso 1 1 calc R U . . .
C22 C 0.531(2) 0.393(2) 0.6147(12) 0.088(8) Uani 0.70(2) 1 d D U P A 1
H22A H 0.5542 0.3982 0.6590 0.105 Uiso 0.70(2) 1 calc R U P A 1
H22B H 0.5329 0.3196 0.5984 0.105 Uiso 0.70(2) 1 calc R U P A 1
C23 C 0.629(3) 0.462(3) 0.5892(15) 0.106(10) Uani 0.70(2) 1 d D U P A 1
H23A H 0.7173 0.4416 0.6000 0.159 Uiso 0.70(2) 1 calc R U P A 1
H23B H 0.6050 0.4563 0.5454 0.159 Uiso 0.70(2) 1 calc R U P A 1
H23C H 0.6262 0.5345 0.6057 0.159 Uiso 0.70(2) 1 calc R U P A 1
C22' C 0.533(3) 0.449(7) 0.585(2) 0.089(11) Uani 0.30(2) 1 d D U P A 2
H22C H 0.5403 0.5052 0.5591 0.106 Uiso 0.30(2) 1 calc R U P A 2
H22D H 0.5628 0.3858 0.5656 0.106 Uiso 0.30(2) 1 calc R U P A 2
C23' C 0.618(4) 0.481(6) 0.648(3) 0.097(13) Uani 0.30(2) 1 d D U P A 2
H23D H 0.7100 0.4954 0.6436 0.146 Uiso 0.30(2) 1 calc R U P A 2
H23E H 0.5873 0.5440 0.6667 0.146 Uiso 0.30(2) 1 calc R U P A 2
H23F H 0.6097 0.4254 0.6732 0.146 Uiso 0.30(2) 1 calc R U P A 2
C24 C -0.0631(13) 0.9128(13) 0.8868(7) 0.057(4) Uani 1 1 d . . . . .
H24A H -0.0848 0.9854 0.8867 0.069 Uiso 1 1 calc R U . . .
H24B H 0.0312 0.9139 0.9032 0.069 Uiso 1 1 calc R U . . .
C25 C -0.145(2) 0.8575(17) 0.9285(8) 0.093(7) Uani 1 1 d . . . . .
H25A H -0.1252 0.8943 0.9691 0.139 Uiso 1 1 calc R U . . .
H25B H -0.2386 0.8575 0.9130 0.139 Uiso 1 1 calc R U . . .
H25C H -0.1226 0.7860 0.9296 0.139 Uiso 1 1 calc R U . . .
C26 C 0.8086(12) 0.4354(9) 0.8279(6) 0.034(3) Uani 1 1 d . . . . .
C27 C 0.8248(11) 0.4089(9) 0.8905(5) 0.029(3) Uani 1 1 d . . . . .
C28 C 0.8888(13) 0.3167(11) 0.8911(5) 0.038(3) Uani 1 1 d . . . . .
C29 C 0.9209(12) 0.2863(10) 0.8309(5) 0.032(3) Uani 1 1 d . . . . .
C30 C 0.8739(11) 0.3626(9) 0.7930(5) 0.027(3) Uani 1 1 d . . . . .
C31 C 0.9013(15) 0.3730(12) 0.7289(6) 0.051(4) Uani 1 1 d . . . . .
H31A H 0.8578 0.4312 0.7134 0.076 Uiso 1 1 calc R U . . .
H31B H 0.9960 0.3853 0.7297 0.076 Uiso 1 1 calc R U . . .
H31C H 0.8675 0.3091 0.7029 0.076 Uiso 1 1 calc R U . . .
C32 C 1.0018(14) 0.1993(11) 0.8149(7) 0.053(4) Uani 1 1 d . . . . .
H32A H 1.0197 0.1593 0.8491 0.079 Uiso 1 1 calc R U . . .
H32B H 0.9534 0.1539 0.7803 0.079 Uiso 1 1 calc R U . . .
H32C H 1.0848 0.2281 0.8050 0.079 Uiso 1 1 calc R U . . .
C33 C 0.9332(17) 0.2622(14) 0.9456(7) 0.065(5) Uani 1 1 d . . . . .
H33A H 0.9747 0.2003 0.9333 0.098 Uiso 1 1 calc R U . . .
H33B H 0.9964 0.3089 0.9746 0.098 Uiso 1 1 calc R U . . .
H33C H 0.8572 0.2420 0.9640 0.098 Uiso 1 1 calc R U . . .
C34 C 0.7963(16) 0.4759(14) 0.9434(7) 0.069(5) Uani 1 1 d . . . . .
H34A H 0.7510 0.5345 0.9296 0.104 Uiso 1 1 calc R U . . .
H34B H 0.7405 0.4354 0.9654 0.104 Uiso 1 1 calc R U . . .
H34C H 0.8788 0.5017 0.9698 0.104 Uiso 1 1 calc R U . . .
C35 C 0.7527(15) 0.5344(11) 0.8076(8) 0.054(4) Uani 1 1 d . . . . .
H35A H 0.7139 0.5691 0.8399 0.081 Uiso 1 1 calc R U . . .
H35B H 0.8234 0.5809 0.7980 0.081 Uiso 1 1 calc R U . . .
H35C H 0.6853 0.5163 0.7720 0.081 Uiso 1 1 calc R U . . .
C36 C 0.5085(12) 0.3128(10) 0.8062(5) 0.031(3) Uani 1 1 d . . . . .
C37 C 0.3028(13) 0.3075(12) 0.7471(6) 0.047(4) Uani 1 1 d . . . . .
H37 H 0.2332 0.2907 0.7143 0.056 Uiso 1 1 calc R U . . .
C38 C 0.2997(13) 0.3661(12) 0.7986(6) 0.047(4) Uani 1 1 d . . . . .
H38 H 0.2269 0.3998 0.8087 0.056 Uiso 1 1 calc R U . . .
C39 C 0.4942(12) 0.2117(11) 0.7126(5) 0.036(3) Uani 1 1 d . U . . .
C40 C 0.6286(11) 0.2003(9) 0.7354(5) 0.024(2) Uani 1 1 d . U . . .
C41 C 0.6967(12) 0.1391(10) 0.6982(5) 0.032(3) Uani 1 1 d . U . . .
H41 H 0.7856 0.1285 0.7116 0.038 Uiso 1 1 calc R U . . .
C42 C 0.6326(13) 0.0930(11) 0.6405(5) 0.038(3) Uani 1 1 d . U . . .
C43 C 0.4986(14) 0.1027(13) 0.6196(6) 0.054(4) Uani 1 1 d . U . . .
H43 H 0.4573 0.0690 0.5817 0.065 Uiso 1 1 calc R U . . .
C44 C 0.4277(15) 0.1625(13) 0.6554(6) 0.057(4) Uani 1 1 d . U . . .
H44 H 0.3379 0.1703 0.6422 0.068 Uiso 1 1 calc R U . . .
C45 C 0.6956(13) 0.0390(11) 0.5388(5) 0.042(3) Uani 1 1 d . . . . .
H45 H 0.6419 0.0793 0.5144 0.050 Uiso 1 1 calc R U . . .
C46 C 0.7812(14) -0.0306(11) 0.5207(5) 0.042(3) Uani 1 1 d . . . . .
H46 H 0.7989 -0.0477 0.4813 0.050 Uiso 1 1 calc R U . . .
C47 C 0.9245(18) -0.1527(14) 0.5778(7) 0.066(5) Uani 1 1 d . . . . .
H47A H 0.8833 -0.2090 0.5968 0.079 Uiso 1 1 calc R U . . .
H47B H 0.9366 -0.1815 0.5373 0.079 Uiso 1 1 calc R U . . .
C48 C 1.0556(19) -0.1163(17) 0.6141(11) 0.099(7) Uani 1 1 d . . . . .
H48A H 1.1102 -0.1742 0.6164 0.148 Uiso 1 1 calc R U . . .
H48B H 1.0980 -0.0615 0.5951 0.148 Uiso 1 1 calc R U . . .
H48C H 1.0446 -0.0890 0.6546 0.148 Uiso 1 1 calc R U . . .
C49 C 0.4515(13) 0.4106(13) 0.8992(6) 0.052(4) Uani 1 1 d . . . . .
H49A H 0.4376 0.4850 0.9029 0.062 Uiso 1 1 calc R U . . .
H49B H 0.5447 0.4044 0.9151 0.062 Uiso 1 1 calc R U . . .
C50 C 0.365(2) 0.3544(17) 0.9373(7) 0.096(7) Uani 1 1 d . . . . .
H50A H 0.3868 0.3850 0.9792 0.144 Uiso 1 1 calc R U . . .
H50B H 0.2722 0.3616 0.9223 0.144 Uiso 1 1 calc R U . . .
H50C H 0.3794 0.2809 0.9346 0.144 Uiso 1 1 calc R U . . .
N1 N 0.3949(17) 0.4295(14) 0.5962(7) 0.093(5) Uani 1 1 d D U . . .
N2 N 0.3485(17) 0.4891(14) 0.6390(7) 0.090(5) Uani 1 1 d . U . . .
N3 N 0.2234(14) 0.4977(9) 0.6163(5) 0.054(3) Uani 1 1 d . U . . .
C20 C 0.191(2) 0.4415(14) 0.5603(8) 0.078(5) Uani 1 1 d . U . . .
H20 H 0.1081 0.4329 0.5353 0.093 Uiso 1 1 calc R U . . .
C21 C 0.301(2) 0.4014(15) 0.5481(9) 0.080(5) Uani 1 1 d . U . . .
H21 H 0.3105 0.3608 0.5122 0.096 Uiso 1 1 calc R U . . .
N4 N -0.0726(9) 0.7572(8) 0.7446(4) 0.031(2) Uani 1 1 d . . . . .
N5 N -0.0867(10) 0.8628(9) 0.8253(5) 0.039(3) Uani 1 1 d . . . . .
N6 N 0.8340(12) -0.0687(10) 0.5719(5) 0.050(3) Uani 1 1 d . . . . .
N7 N 0.7862(13) -0.0304(9) 0.6215(5) 0.046(3) Uani 1 1 d . . . . .
N8 N 0.7059(10) 0.0366(9) 0.6000(4) 0.035(3) Uani 1 1 d . . . . .
N9 N 0.4312(10) 0.2756(9) 0.7516(4) 0.036(3) Uani 1 1 d . . . . .
N10 N 0.4242(10) 0.3692(8) 0.8358(4) 0.035(2) Uani 1 1 d . . . . .
I1 I 0.12772(9) 0.61253(7) 0.87584(4) 0.0413(2) Uani 1 1 d . . . . .
I2 I 0.62249(9) 0.10541(7) 0.86869(4) 0.0420(2) Uani 1 1 d . . . . .
I3 I 0.50356(13) -0.24219(10) 0.56334(5) 0.0731(4) Uani 1 1 d . . . . .
I4 I -0.03831(10) 0.80568(9) 0.39927(4) 0.0625(3) Uani 1 1 d . . . . .
Ir1 Ir 0.19310(5) 0.77854(4) 0.81730(2) 0.02418(14) Uani 1 1 d . . . . .
Ir2 Ir 0.69898(5) 0.28068(4) 0.82037(2) 0.02215(14) Uani 1 1 d . . . . .
O1 O 0.145(2) 0.6467(14) 0.4955(10) 0.139(7) Uani 1 1 d D . . . .
H1A H 0.20(2) 0.678(16) 0.526(8) 0.167 Uiso 1 1 d D U . . .
H1B H 0.12(3) 0.693(13) 0.473(9) 0.167 Uiso 1 1 d D U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.406(17) . ?
C1 C5 1.425(17) . ?
C1 C10 1.503(16) . ?
C1 Ir1 2.190(11) . ?
C2 C3 1.450(19) . ?
C2 C9 1.48(2) . ?
C2 Ir1 2.249(13) . ?
C3 C4 1.39(2) . ?
C3 C8 1.49(2) . ?
C3 Ir1 2.288(12) . ?
C4 C5 1.44(2) . ?
C4 C7 1.496(19) . ?
C4 Ir1 2.283(11) . ?
C5 C6 1.50(2) . ?
C5 Ir1 2.165(12) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 N5 1.360(15) . ?
C11 N4 1.369(14) . ?
C11 Ir1 2.003(13) . ?
C12 C13 1.338(19) . ?
C12 N5 1.403(16) . ?
C12 H12 0.9300 . ?
C13 N4 1.375(16) . ?
C13 H13 0.9300 . ?
C14 C19 1.376(16) . ?
C14 N4 1.398(15) . ?
C14 C15 1.413(16) . ?
C15 C16 1.377(16) . ?
C15 Ir1 2.057(11) . ?
C16 C17 1.377(16) . ?
C16 H16 0.9300 . ?
C17 C18 1.393(19) . ?
C17 N3 1.434(17) . ?
C18 C19 1.382(19) . ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?
C22 C23 1.495(19) . ?
C22 N1 1.509(18) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C22' N1 1.47(2) . ?
C22' C23' 1.52(2) . ?
C22' H22C 0.9700 . ?
C22' H22D 0.9700 . ?
C23' H23D 0.9600 . ?
C23' H23E 0.9600 . ?
C23' H23F 0.9600 . ?
C24 N5 1.428(16) . ?
C24 C25 1.53(2) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 C30 1.421(16) . ?
C26 C27 1.455(17) . ?
C26 C35 1.507(18) . ?
C26 Ir2 2.171(11) . ?
C27 C28 1.389(18) . ?
C27 C34 1.465(17) . ?
C27 Ir2 2.303(10) . ?
C28 C29 1.451(17) . ?
C28 C33 1.485(18) . ?
C28 Ir2 2.277(12) . ?
C29 C30 1.415(17) . ?
C29 C32 1.480(18) . ?
C29 Ir2 2.225(12) . ?
C30 C31 1.512(16) . ?
C30 Ir2 2.192(11) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 N9 1.361(14) . ?
C36 N10 1.366(15) . ?
C36 Ir2 1.992(13) . ?
C37 C38 1.313(18) . ?
C37 N9 1.387(16) . ?
C37 H37 0.9300 . ?
C38 N10 1.394(16) . ?
C38 H38 0.9300 . ?
C39 N9 1.394(15) . ?
C39 C40 1.404(16) . ?
C39 C44 1.409(16) . ?
C40 C41 1.382(15) . ?
C40 Ir2 2.056(10) . ?
C41 C42 1.397(15) . ?
C41 H41 0.9300 . ?
C42 C43 1.388(18) . ?
C42 N8 1.431(15) . ?
C43 C44 1.371(19) . ?
C43 H43 0.9300 . ?
C44 H44 0.9300 . ?
C45 N8 1.353(15) . ?
C45 C46 1.367(19) . ?
C45 H45 0.9300 . ?
C46 N6 1.336(16) . ?
C46 H46 0.9300 . ?
C47 C48 1.46(2) . ?
C47 N6 1.468(19) . ?
C47 H47A 0.9700 . ?
C47 H47B 0.9700 . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 0.9600 . ?
C49 N10 1.433(14) . ?
C49 C50 1.51(2) . ?
C49 H49A 0.9700 . ?
C49 H49B 0.9700 . ?
C50 H50A 0.9600 . ?
C50 H50B 0.9600 . ?
C50 H50C 0.9600 . ?
N1 C21 1.32(2) . ?
N1 N2 1.326(18) . ?
N2 N3 1.31(2) . ?
N3 C20 1.354(19) . ?
C20 C21 1.31(3) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
N6 N7 1.337(14) . ?
N7 N8 1.302(15) . ?
I1 Ir1 2.6908(9) . ?
I2 Ir2 2.6921(9) . ?
O1 H1A 0.85(2) . ?
O1 H1B 0.85(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C5 108.6(11) . . ?
C2 C1 C10 125.5(12) . . ?
C5 C1 C10 125.5(13) . . ?
C2 C1 Ir1 73.8(7) . . ?
C5 C1 Ir1 70.0(7) . . ?
C10 C1 Ir1 128.1(9) . . ?
C1 C2 C3 107.1(12) . . ?
C1 C2 C9 129.0(14) . . ?
C3 C2 C9 123.8(14) . . ?
C1 C2 Ir1 69.3(7) . . ?
C3 C2 Ir1 72.8(7) . . ?
C9 C2 Ir1 125.3(10) . . ?
C4 C3 C2 108.8(12) . . ?
C4 C3 C8 126.0(16) . . ?
C2 C3 C8 125.0(17) . . ?
C4 C3 Ir1 72.1(7) . . ?
C2 C3 Ir1 69.9(7) . . ?
C8 C3 Ir1 127.9(10) . . ?
C3 C4 C5 107.9(12) . . ?
C3 C4 C7 125.8(16) . . ?
C5 C4 C7 125.5(17) . . ?
C3 C4 Ir1 72.5(7) . . ?
C5 C4 Ir1 66.7(6) . . ?
C7 C4 Ir1 133.9(10) . . ?
C1 C5 C4 107.4(12) . . ?
C1 C5 C6 126.1(15) . . ?
C4 C5 C6 125.3(15) . . ?
C1 C5 Ir1 71.8(7) . . ?
C4 C5 Ir1 75.6(8) . . ?
C6 C5 Ir1 127.6(10) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C3 C8 H8A 109.5 . . ?
C3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C2 C9 H9A 109.5 . . ?
C2 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C2 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C1 C10 H10A 109.5 . . ?
C1 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C1 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N5 C11 N4 105.2(10) . . ?
N5 C11 Ir1 137.3(9) . . ?
N4 C11 Ir1 117.5(9) . . ?
C13 C12 N5 107.1(12) . . ?
C13 C12 H12 126.4 . . ?
N5 C12 H12 126.4 . . ?
C12 C13 N4 107.6(12) . . ?
C12 C13 H13 126.2 . . ?
N4 C13 H13 126.2 . . ?
C19 C14 N4 123.9(11) . . ?
C19 C14 C15 123.5(12) . . ?
N4 C14 C15 112.6(9) . . ?
C16 C15 C14 115.9(10) . . ?
C16 C15 Ir1 128.3(9) . . ?
C14 C15 Ir1 115.8(8) . . ?
C15 C16 C17 120.7(13) . . ?
C15 C16 H16 119.6 . . ?
C17 C16 H16 119.6 . . ?
C16 C17 C18 122.9(12) . . ?
C16 C17 N3 118.5(13) . . ?
C18 C17 N3 118.6(12) . . ?
C19 C18 C17 117.3(11) . . ?
C19 C18 H18 121.3 . . ?
C17 C18 H18 121.3 . . ?
C14 C19 C18 119.5(12) . . ?
C14 C19 H19 120.2 . . ?
C18 C19 H19 120.2 . . ?
C23 C22 N1 106.8(19) . . ?
C23 C22 H22A 110.4 . . ?
N1 C22 H22A 110.4 . . ?
C23 C22 H22B 110.4 . . ?
N1 C22 H22B 110.4 . . ?
H22A C22 H22B 108.6 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N1 C22' C23' 106(2) . . ?
N1 C22' H22C 110.6 . . ?
C23' C22' H22C 110.6 . . ?
N1 C22' H22D 110.6 . . ?
C23' C22' H22D 110.6 . . ?
H22C C22' H22D 108.7 . . ?
C22' C23' H23D 109.5 . . ?
C22' C23' H23E 109.5 . . ?
H23D C23' H23E 109.5 . . ?
C22' C23' H23F 109.5 . . ?
H23D C23' H23F 109.5 . . ?
H23E C23' H23F 109.5 . . ?
N5 C24 C25 113.1(13) . . ?
N5 C24 H24A 109.0 . . ?
C25 C24 H24A 109.0 . . ?
N5 C24 H24B 109.0 . . ?
C25 C24 H24B 109.0 . . ?
H24A C24 H24B 107.8 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C30 C26 C27 108.4(11) . . ?
C30 C26 C35 126.5(12) . . ?
C27 C26 C35 124.4(12) . . ?
C30 C26 Ir2 71.8(6) . . ?
C27 C26 Ir2 76.0(7) . . ?
C35 C26 Ir2 126.2(9) . . ?
C28 C27 C26 106.6(10) . . ?
C28 C27 C34 127.3(12) . . ?
C26 C27 C34 125.5(13) . . ?
C28 C27 Ir2 71.3(6) . . ?
C26 C27 Ir2 66.2(6) . . ?
C34 C27 Ir2 133.8(9) . . ?
C27 C28 C29 109.7(11) . . ?
C27 C28 C33 126.4(12) . . ?
C29 C28 C33 123.5(13) . . ?
C27 C28 Ir2 73.4(7) . . ?
C29 C28 Ir2 69.3(6) . . ?
C33 C28 Ir2 128.9(10) . . ?
C30 C29 C28 106.9(11) . . ?
C30 C29 C32 126.9(12) . . ?
C28 C29 C32 125.8(12) . . ?
C30 C29 Ir2 70.1(7) . . ?
C28 C29 Ir2 73.1(7) . . ?
C32 C29 Ir2 127.4(8) . . ?
C29 C30 C26 108.1(10) . . ?
C29 C30 C31 126.2(11) . . ?
C26 C30 C31 125.3(12) . . ?
C29 C30 Ir2 72.6(7) . . ?
C26 C30 Ir2 70.2(6) . . ?
C31 C30 Ir2 128.0(8) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C29 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C29 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C28 C33 H33A 109.5 . . ?
C28 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C28 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C27 C34 H34A 109.5 . . ?
C27 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C27 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C26 C35 H35A 109.5 . . ?
C26 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C26 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
N9 C36 N10 103.1(10) . . ?
N9 C36 Ir2 118.4(8) . . ?
N10 C36 Ir2 138.3(8) . . ?
C38 C37 N9 105.9(11) . . ?
C38 C37 H37 127.0 . . ?
N9 C37 H37 127.0 . . ?
C37 C38 N10 108.5(12) . . ?
C37 C38 H38 125.8 . . ?
N10 C38 H38 125.8 . . ?
N9 C39 C40 114.4(10) . . ?
N9 C39 C44 122.5(11) . . ?
C40 C39 C44 123.1(11) . . ?
C41 C40 C39 116.9(10) . . ?
C41 C40 Ir2 128.5(8) . . ?
C39 C40 Ir2 114.6(8) . . ?
C40 C41 C42 120.2(11) . . ?
C40 C41 H41 119.9 . . ?
C42 C41 H41 119.9 . . ?
C43 C42 C41 121.9(12) . . ?
C43 C42 N8 117.8(10) . . ?
C41 C42 N8 120.3(11) . . ?
C44 C43 C42 119.5(11) . . ?
C44 C43 H43 120.3 . . ?
C42 C43 H43 120.3 . . ?
C43 C44 C39 118.3(13) . . ?
C43 C44 H44 120.8 . . ?
C39 C44 H44 120.8 . . ?
N8 C45 C46 105.1(12) . . ?
N8 C45 H45 127.5 . . ?
C46 C45 H45 127.5 . . ?
N6 C46 C45 104.9(11) . . ?
N6 C46 H46 127.6 . . ?
C45 C46 H46 127.6 . . ?
C48 C47 N6 113.2(15) . . ?
C48 C47 H47A 108.9 . . ?
N6 C47 H47A 108.9 . . ?
C48 C47 H47B 108.9 . . ?
N6 C47 H47B 108.9 . . ?
H47A C47 H47B 107.8 . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
N10 C49 C50 112.8(12) . . ?
N10 C49 H49A 109.0 . . ?
C50 C49 H49A 109.0 . . ?
N10 C49 H49B 109.0 . . ?
C50 C49 H49B 109.0 . . ?
H49A C49 H49B 107.8 . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C21 N1 N2 110.9(17) . . ?
C21 N1 C22' 117(2) . . ?
N2 N1 C22' 121(3) . . ?
C21 N1 C22 132.1(18) . . ?
N2 N1 C22 116.1(18) . . ?
N3 N2 N1 105.3(14) . . ?
N2 N3 C20 109.8(14) . . ?
N2 N3 C17 120.9(12) . . ?
C20 N3 C17 129.3(15) . . ?
C21 C20 N3 106.8(18) . . ?
C21 C20 H20 126.6 . . ?
N3 C20 H20 126.6 . . ?
C20 C21 N1 107.1(16) . . ?
C20 C21 H21 126.5 . . ?
N1 C21 H21 126.5 . . ?
C11 N4 C13 110.4(11) . . ?
C11 N4 C14 116.2(10) . . ?
C13 N4 C14 133.4(10) . . ?
C11 N5 C12 109.6(11) . . ?
C11 N5 C24 125.5(11) . . ?
C12 N5 C24 124.3(11) . . ?
C46 N6 N7 113.5(12) . . ?
C46 N6 C47 127.6(12) . . ?
N7 N6 C47 118.6(12) . . ?
N8 N7 N6 102.7(10) . . ?
N7 N8 C45 113.7(11) . . ?
N7 N8 C42 119.0(10) . . ?
C45 N8 C42 127.1(12) . . ?
C36 N9 C37 112.3(10) . . ?
C36 N9 C39 114.6(10) . . ?
C37 N9 C39 133.1(10) . . ?
C36 N10 C38 110.2(10) . . ?
C36 N10 C49 124.8(10) . . ?
C38 N10 C49 124.3(10) . . ?
C11 Ir1 C15 77.7(5) . . ?
C11 Ir1 C5 103.3(5) . . ?
C15 Ir1 C5 118.6(5) . . ?
C11 Ir1 C1 130.1(5) . . ?
C15 Ir1 C1 94.8(4) . . ?
C5 Ir1 C1 38.2(5) . . ?
C11 Ir1 C2 165.8(5) . . ?
C15 Ir1 C2 106.0(5) . . ?
C5 Ir1 C2 62.7(5) . . ?
C1 Ir1 C2 36.9(5) . . ?
C11 Ir1 C4 109.9(5) . . ?
C15 Ir1 C4 155.5(5) . . ?
C5 Ir1 C4 37.7(5) . . ?
C1 Ir1 C4 62.2(4) . . ?
C2 Ir1 C4 61.2(5) . . ?
C11 Ir1 C3 140.3(5) . . ?
C15 Ir1 C3 142.0(5) . . ?
C5 Ir1 C3 61.8(6) . . ?
C1 Ir1 C3 61.7(5) . . ?
C2 Ir1 C3 37.3(5) . . ?
C4 Ir1 C3 35.3(5) . . ?
C11 Ir1 I1 90.1(3) . . ?
C15 Ir1 I1 87.6(3) . . ?
C5 Ir1 I1 152.3(4) . . ?
C1 Ir1 I1 139.3(3) . . ?
C2 Ir1 I1 103.6(4) . . ?
C4 Ir1 I1 115.0(4) . . ?
C3 Ir1 I1 92.5(4) . . ?
C36 Ir2 C40 77.8(4) . . ?
C36 Ir2 C26 103.0(5) . . ?
C40 Ir2 C26 119.7(5) . . ?
C36 Ir2 C30 129.1(5) . . ?
C40 Ir2 C30 95.1(4) . . ?
C26 Ir2 C30 38.0(4) . . ?
C36 Ir2 C29 165.6(5) . . ?
C40 Ir2 C29 105.4(4) . . ?
C26 Ir2 C29 63.0(5) . . ?
C30 Ir2 C29 37.4(4) . . ?
C36 Ir2 C28 140.7(5) . . ?
C40 Ir2 C28 141.5(5) . . ?
C26 Ir2 C28 61.6(5) . . ?
C30 Ir2 C28 62.0(4) . . ?
C29 Ir2 C28 37.6(4) . . ?
C36 Ir2 C27 110.0(4) . . ?
C40 Ir2 C27 156.5(4) . . ?
C26 Ir2 C27 37.8(4) . . ?
C30 Ir2 C27 62.5(4) . . ?
C29 Ir2 C27 61.7(4) . . ?
C28 Ir2 C27 35.3(4) . . ?
C36 Ir2 I2 88.8(3) . . ?
C40 Ir2 I2 87.8(3) . . ?
C26 Ir2 I2 151.6(3) . . ?
C30 Ir2 I2 141.7(3) . . ?
C29 Ir2 I2 105.2(3) . . ?
C28 Ir2 I2 92.9(3) . . ?
C27 Ir2 I2 114.0(3) . . ?
H1A O1 H1B 107(4) . . ?

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
C5 C1 C2 C3 -1.7(14) . . . . ?
C10 C1 C2 C3 171.0(12) . . . . ?
Ir1 C1 C2 C3 -63.4(9) . . . . ?
C5 C1 C2 C9 -179.0(13) . . . . ?
C10 C1 C2 C9 -6(2) . . . . ?
Ir1 C1 C2 C9 119.3(14) . . . . ?
C5 C1 C2 Ir1 61.7(8) . . . . ?
C10 C1 C2 Ir1 -125.6(12) . . . . ?
C1 C2 C3 C4 -0.9(14) . . . . ?
C9 C2 C3 C4 176.5(12) . . . . ?
Ir1 C2 C3 C4 -62.0(9) . . . . ?
C1 C2 C3 C8 -176.0(13) . . . . ?
C9 C2 C3 C8 1(2) . . . . ?
Ir1 C2 C3 C8 122.9(14) . . . . ?
C1 C2 C3 Ir1 61.1(8) . . . . ?
C9 C2 C3 Ir1 -121.4(13) . . . . ?
C2 C3 C4 C5 3.1(15) . . . . ?
C8 C3 C4 C5 178.2(13) . . . . ?
Ir1 C3 C4 C5 -57.5(8) . . . . ?
C2 C3 C4 C7 -167.3(13) . . . . ?
C8 C3 C4 C7 8(2) . . . . ?
Ir1 C3 C4 C7 132.0(14) . . . . ?
C2 C3 C4 Ir1 60.6(9) . . . . ?
C8 C3 C4 Ir1 -124.3(14) . . . . ?
C2 C1 C5 C4 3.6(13) . . . . ?
C10 C1 C5 C4 -169.1(12) . . . . ?
Ir1 C1 C5 C4 67.8(8) . . . . ?
C2 C1 C5 C6 172.0(13) . . . . ?
C10 C1 C5 C6 -1(2) . . . . ?
Ir1 C1 C5 C6 -123.8(14) . . . . ?
C2 C1 C5 Ir1 -64.2(8) . . . . ?
C10 C1 C5 Ir1 123.1(12) . . . . ?
C3 C4 C5 C1 -4.1(14) . . . . ?
C7 C4 C5 C1 166.4(12) . . . . ?
Ir1 C4 C5 C1 -65.3(8) . . . . ?
C3 C4 C5 C6 -172.7(13) . . . . ?
C7 C4 C5 C6 -2(2) . . . . ?
Ir1 C4 C5 C6 126.1(14) . . . . ?
C3 C4 C5 Ir1 61.1(9) . . . . ?
C7 C4 C5 Ir1 -128.4(13) . . . . ?
N5 C12 C13 N4 -0.2(16) . . . . ?
C19 C14 C15 C16 0.9(17) . . . . ?
N4 C14 C15 C16 -179.6(10) . . . . ?
C19 C14 C15 Ir1 -179.2(9) . . . . ?
N4 C14 C15 Ir1 0.2(13) . . . . ?
C14 C15 C16 C17 2.1(17) . . . . ?
Ir1 C15 C16 C17 -177.8(9) . . . . ?
C15 C16 C17 C18 -3.8(19) . . . . ?
C15 C16 C17 N3 175.5(11) . . . . ?
C16 C17 C18 C19 2(2) . . . . ?
N3 C17 C18 C19 -177.0(12) . . . . ?
N4 C14 C19 C18 178.3(12) . . . . ?
C15 C14 C19 C18 -2.4(19) . . . . ?
C17 C18 C19 C14 0.7(19) . . . . ?
C30 C26 C27 C28 -4.8(13) . . . . ?
C35 C26 C27 C28 -175.2(12) . . . . ?
Ir2 C26 C27 C28 60.2(8) . . . . ?
C30 C26 C27 C34 167.0(12) . . . . ?
C35 C26 C27 C34 -3(2) . . . . ?
Ir2 C26 C27 C34 -127.9(13) . . . . ?
C30 C26 C27 Ir2 -65.0(8) . . . . ?
C35 C26 C27 Ir2 124.6(12) . . . . ?
C26 C27 C28 C29 3.1(13) . . . . ?
C34 C27 C28 C29 -168.6(13) . . . . ?
Ir2 C27 C28 C29 60.0(8) . . . . ?
C26 C27 C28 C33 176.6(13) . . . . ?
C34 C27 C28 C33 5(2) . . . . ?
Ir2 C27 C28 C33 -126.5(14) . . . . ?
C26 C27 C28 Ir2 -56.9(8) . . . . ?
C34 C27 C28 Ir2 131.4(14) . . . . ?
C27 C28 C29 C30 -0.2(14) . . . . ?
C33 C28 C29 C30 -174.0(12) . . . . ?
Ir2 C28 C29 C30 62.3(8) . . . . ?
C27 C28 C29 C32 173.1(12) . . . . ?
C33 C28 C29 C32 -1(2) . . . . ?
Ir2 C28 C29 C32 -124.4(12) . . . . ?
C27 C28 C29 Ir2 -62.6(9) . . . . ?
C33 C28 C29 Ir2 123.7(13) . . . . ?
C28 C29 C30 C26 -2.8(13) . . . . ?
C32 C29 C30 C26 -176.0(11) . . . . ?
Ir2 C29 C30 C26 61.5(8) . . . . ?
C28 C29 C30 C31 170.9(12) . . . . ?
C32 C29 C30 C31 -2.3(19) . . . . ?
Ir2 C29 C30 C31 -124.8(12) . . . . ?
C28 C29 C30 Ir2 -64.4(8) . . . . ?
C32 C29 C30 Ir2 122.4(12) . . . . ?
C27 C26 C30 C29 4.7(13) . . . . ?
C35 C26 C30 C29 174.9(11) . . . . ?
Ir2 C26 C30 C29 -63.1(8) . . . . ?
C27 C26 C30 C31 -169.0(11) . . . . ?
C35 C26 C30 C31 1.1(19) . . . . ?
Ir2 C26 C30 C31 123.2(12) . . . . ?
C27 C26 C30 Ir2 67.8(8) . . . . ?
C35 C26 C30 Ir2 -122.0(12) . . . . ?
N9 C37 C38 N10 -1.3(17) . . . . ?
N9 C39 C40 C41 -179.0(11) . . . . ?
C44 C39 C40 C41 1(2) . . . . ?
N9 C39 C40 Ir2 -0.1(15) . . . . ?
C44 C39 C40 Ir2 -179.7(12) . . . . ?
C39 C40 C41 C42 0.9(18) . . . . ?
Ir2 C40 C41 C42 -177.8(10) . . . . ?
C40 C41 C42 C43 -3(2) . . . . ?
C40 C41 C42 N8 175.1(12) . . . . ?
C41 C42 C43 C44 3(2) . . . . ?
N8 C42 C43 C44 -175.4(15) . . . . ?
C42 C43 C44 C39 0(2) . . . . ?
N9 C39 C44 C43 178.7(14) . . . . ?
C40 C39 C44 C43 -2(2) . . . . ?
N8 C45 C46 N6 0.4(15) . . . . ?
C23' C22' N1 C21 179(5) . . . . ?
C23' C22' N1 N2 38(7) . . . . ?
C23 C22 N1 C21 91(3) . . . . ?
C23 C22 N1 N2 -101(2) . . . . ?
C21 N1 N2 N3 0(2) . . . . ?
C22' N1 N2 N3 144(4) . . . . ?
C22 N1 N2 N3 -170.6(17) . . . . ?
N1 N2 N3 C20 2(2) . . . . ?
N1 N2 N3 C17 -178.1(14) . . . . ?
C16 C17 N3 N2 4(2) . . . . ?
C18 C17 N3 N2 -177.0(15) . . . . ?
C16 C17 N3 C20 -175.8(15) . . . . ?
C18 C17 N3 C20 4(2) . . . . ?
N2 N3 C20 C21 -2(2) . . . . ?
C17 N3 C20 C21 177.2(15) . . . . ?
N3 C20 C21 N1 2(2) . . . . ?
N2 N1 C21 C20 -1(3) . . . . ?
C22' N1 C21 C20 -147(4) . . . . ?
C22 N1 C21 C20 167(2) . . . . ?
N5 C11 N4 C13 1.8(14) . . . . ?
Ir1 C11 N4 C13 -175.9(9) . . . . ?
N5 C11 N4 C14 -176.5(10) . . . . ?
Ir1 C11 N4 C14 5.8(13) . . . . ?
C12 C13 N4 C11 -1.0(15) . . . . ?
C12 C13 N4 C14 176.9(13) . . . . ?
C19 C14 N4 C11 175.7(11) . . . . ?
C15 C14 N4 C11 -3.8(15) . . . . ?
C19 C14 N4 C13 -2(2) . . . . ?
C15 C14 N4 C13 178.4(13) . . . . ?
N4 C11 N5 C12 -1.9(14) . . . . ?
Ir1 C11 N5 C12 175.1(11) . . . . ?
N4 C11 N5 C24 169.3(13) . . . . ?
Ir1 C11 N5 C24 -14(2) . . . . ?
C13 C12 N5 C11 1.4(16) . . . . ?
C13 C12 N5 C24 -170.0(14) . . . . ?
C25 C24 N5 C11 -107.0(16) . . . . ?
C25 C24 N5 C12 63(2) . . . . ?
C45 C46 N6 N7 1.4(16) . . . . ?
C45 C46 N6 C47 174.8(15) . . . . ?
C48 C47 N6 C46 117.3(18) . . . . ?
C48 C47 N6 N7 -70(2) . . . . ?
C46 N6 N7 N8 -2.7(15) . . . . ?
C47 N6 N7 N8 -176.6(13) . . . . ?
N6 N7 N8 C45 2.9(14) . . . . ?
N6 N7 N8 C42 178.8(10) . . . . ?
C46 C45 N8 N7 -2.2(15) . . . . ?
C46 C45 N8 C42 -177.7(12) . . . . ?
C43 C42 N8 N7 -136.5(14) . . . . ?
C41 C42 N8 N7 45.4(18) . . . . ?
C43 C42 N8 C45 39(2) . . . . ?
C41 C42 N8 C45 -139.3(14) . . . . ?
N10 C36 N9 C37 -0.1(14) . . . . ?
Ir2 C36 N9 C37 -177.5(9) . . . . ?
N10 C36 N9 C39 -178.3(11) . . . . ?
Ir2 C36 N9 C39 4.3(15) . . . . ?
C38 C37 N9 C36 0.9(17) . . . . ?
C38 C37 N9 C39 178.7(14) . . . . ?
C40 C39 N9 C36 -2.6(17) . . . . ?
C44 C39 N9 C36 177.1(13) . . . . ?
C40 C39 N9 C37 179.7(14) . . . . ?
C44 C39 N9 C37 -1(2) . . . . ?
N9 C36 N10 C38 -0.7(14) . . . . ?
Ir2 C36 N10 C38 175.9(11) . . . . ?
N9 C36 N10 C49 169.7(12) . . . . ?
Ir2 C36 N10 C49 -14(2) . . . . ?
C37 C38 N10 C36 1.3(17) . . . . ?
C37 C38 N10 C49 -169.1(14) . . . . ?
C50 C49 N10 C36 -110.1(16) . . . . ?
C50 C49 N10 C38 59(2) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C22' H22C I3 0.97 3.27 4.05(9) 138.5 1_565
C22' H22D I3 0.97 3.20 3.97(6) 138.2 2_656
C37 H37 I4 0.93 3.05 3.958(13) 167.5 2_566
C38 H38 I1 0.93 3.27 4.078(14) 145.9 .
C44 H44 I4 0.93 3.09 4.017(14) 178.8 2_566
C45 H45 I3 0.93 3.15 4.069(15) 171.4 2_656
C46 H46 I4 0.93 3.21 4.007(13) 144.6 1_645
C47 H47B I4 0.97 3.11 4.038(16) 160.2 1_645
C21 H21 I3 0.93 3.10 3.922(17) 148.2 2_656
O1 H1A I3 0.85(2) 3.13(19) 3.822(19) 140(25) 1_565

_refine_diff_density_max         2.548
_refine_diff_density_min         -2.479
_refine_diff_density_rms         0.208



# start Validation Reply Form
_vrf_PLAT420_PR15                
;
PROBLEM: D-H Without Acceptor       O1     --  H1A    ...     Please Check 
RESPONSE: There is no acceptor in the vicinity of O1...H1A
;
_vrf_PLAT971_PR15                
;
PROBLEM: Check Calcd Residual Density  1.41A From     Ir2       2.69 eA-3  
RESPONSE:  it is a heavy atom stucture. The electron density is near to
the metal
;
_vrf_PLAT972_PR15                
;
PROBLEM: Check Calcd Residual Density  1.49A From      O1      -2.76 eA-3  
RESPONSE: Since it is a heavy atom structure,this may due to absorption error
;
# end Validation Reply Form


