# Supplementary Information (SI) for Catalysis Science & Technology.
# This journal is © The Royal Society of Chemistry 2025

####################################################################### 
# 
# 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_23ma081_absorption_really
_database_code_depnum_ccdc_archive 'CCDC 2394912'
loop_
_audit_author_name
_audit_author_address
'Lorraine Malaspina'
;University of Bern
Switzerland
;
_audit_update_record             
;
2024-10-30 deposited with the CCDC.	2024-12-18 downloaded from the CCDC.
;
_audit_creation_date             2023-11-03
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C11 H11 Cl2 N3 O2 Pd'
_chemical_formula_sum            'C11 H11 Cl2 N3 O2 Pd'
_chemical_formula_weight         394.53
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C96  H88  Cl16  N24  O8  Pd8  '
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 1 2/a 1'
_space_group_name_Hall           '-I 2ya'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   19.6202(3)
_cell_length_b                   9.6407(2)
_cell_length_c                   14.9332(3)
_cell_angle_alpha                90
_cell_angle_beta                 91.131(2)
_cell_angle_gamma                90
_cell_volume                     2824.10(9)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    33186
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      33.4920
_cell_measurement_theta_min      2.3210
_shelx_estimated_absorpt_T_max   0.867
_shelx_estimated_absorpt_T_min   0.787
_exptl_absorpt_coefficient_mu    1.692
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.746
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.90a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.856
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1552
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
27 4 -1 0.0532
-1 13 6 0.0487
-1 -10 14 0.0418
-23 7 4 0.0812
-17 -6 -14 0.0418
22 2 -13 0.0448
-1 1 0 0.0633
0 1 -1 0.0653
-2 -5 19 0.0337
-2 -3 -21 0.0502
20 2 14 0.0422
-13 -4 18 0.0480
18 8 10 0.0399
10 -9 -14 0.0629
-4 4 -20 0.0563
-18 8 -9 0.0680
17 -9 8 0.0448

_exptl_crystal_size_max          0.149
_exptl_crystal_size_mid          0.113
_exptl_crystal_size_min          0.087
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
26.9887 4.0009 -0.9971 -0.5161 -0.6573 -0.5835
-1.0009 12.9969 5.9989 -0.2365 -0.7364 0.6309
-0.9920 -9.9982 13.9958 -0.5220 0.8429 -0.0245
-22.9920 6.9969 3.9972 0.2998 -0.0634 0.9444
-16.9972 -5.9994 -13.9981 0.9114 0.4392 -0.0846
21.9868 2.0013 -12.9945 0.0656 -0.6194 -0.7925
-0.9999 0.9997 -0.0000 0.0190 -0.0496 0.0624
-0.0006 0.9998 -0.9997 0.0383 -0.0775 0.0140
-1.9912 -4.9995 18.9946 -0.7074 0.6049 0.2942
-2.0060 -2.9990 -20.9948 0.8798 -0.0626 -0.5241
19.9972 2.0005 13.9982 -0.9669 -0.2264 -0.1389
-12.9878 -4.0004 17.9940 -0.4449 0.6855 0.5959
17.9949 7.9992 9.9994 -0.7757 -0.6355 0.0418
9.9937 -8.9971 -13.9959 0.3655 0.2432 -0.8995
-4.0067 3.9993 -19.9950 0.8709 -0.4682 -0.1958
-17.9988 7.9973 -8.9989 0.7132 -0.3746 0.5603
16.9990 -8.9971 7.9990 -0.6517 0.4394 -0.5927

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_unetI/netI     0.0145
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            41482
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         2.076
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -9.00  90.00   0.50    1.50    --   13.29  58.00 -74.00  198
  2  ω    -35.00  63.00   0.50    1.50    --  -13.44  58.00 -74.00  196
  3  ω    -90.00   9.00   0.50    1.50    --  -13.44 -58.00 144.00  198
  4  ω    -90.00   8.00   0.50    1.50    --  -13.44 -57.00   0.00  196
  5  ω    -19.00  29.00   0.50    1.50    --  -13.44 -99.00 -90.00   96
  6  ω    -25.00  68.00   0.50    1.50    --  -13.44  19.00 -90.00  186
  7  ω    -19.00  29.00   0.50    1.50    --  -13.44 -99.00  30.00   96
  8  ω    -18.00  55.00   0.50    1.50    --   13.29 -99.00 150.00  146
  9  ω    -18.00  55.00   0.50    1.50    --   13.29 -99.00  30.00  146
 10  ω    -18.00  55.00   0.50    1.50    --   13.29 -99.00-120.00  146
 11  ω    -89.00 -40.00   0.50    1.50    --  -13.44 178.00 -60.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix-Arc 100'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0203827000
_diffrn_orient_matrix_UB_12      -0.0014199000
_diffrn_orient_matrix_UB_13      -0.0397536000
_diffrn_orient_matrix_UB_21      -0.0143687000
_diffrn_orient_matrix_UB_22      -0.0639918000
_diffrn_orient_matrix_UB_23      0.0134962000
_diffrn_orient_matrix_UB_31      -0.0261702000
_diffrn_orient_matrix_UB_32      0.0362401000
_diffrn_orient_matrix_UB_33      0.0222852000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3989
_reflns_number_total             4316
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.824
_refine_diff_density_min         -0.508
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     216
_refine_ls_number_reflns         4316
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0252
_refine_ls_R_factor_gt           0.0222
_refine_ls_restrained_S_all      1.107
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0300P)²+3.6581P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0584
_refine_ls_wR_factor_ref         0.0595
_refine_special_details          ?
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd01 Pd 0.40234(2) 0.51763(2) 0.52134(2) 0.01868(5) Uani 1 1 d . . . . .
Cl1 Cl 0.43466(2) 0.58596(5) 0.38022(3) 0.02752(10) Uani 1 1 d . . . . .
Cl2 Cl 0.38312(3) 0.74089(4) 0.56841(3) 0.03094(10) Uani 1 1 d . . . . .
O1 O 0.43904(8) 0.10713(14) 0.44646(10) 0.0320(3) Uani 1 1 d . . . . .
O2 O 0.38295(9) 0.22155(15) 0.71818(10) 0.0356(3) Uani 1 1 d . . . . .
N1 N 0.41812(7) 0.31844(15) 0.49120(10) 0.0204(3) Uani 1 1 d . . . . .
N2 N 0.37632(8) 0.42797(15) 0.64020(10) 0.0218(3) Uani 1 1 d . . . . .
N3 N 0.37500(8) 0.56458(17) 0.77345(11) 0.0260(3) Uani 1 1 d . . . . .
C5 C 0.34055(9) 0.49000(17) 0.70919(12) 0.0206(3) Uani 1 1 d . . . . .
C9 C 0.27013(9) 0.4774(2) 0.71223(13) 0.0248(3) Uani 1 1 d . . . . .
C4 C 0.38990(9) 0.29082(18) 0.64976(12) 0.0235(3) Uani 1 1 d . . . . .
C3 C 0.41220(9) 0.22990(18) 0.56443(12) 0.0216(3) Uani 1 1 d . . . . .
C1 C 0.43410(10) 0.2424(2) 0.42365(13) 0.0271(4) Uani 1 1 d . . . . .
C8 C 0.23592(11) 0.5407(2) 0.78027(16) 0.0346(4) Uani 1 1 d . . . . .
C2 C 0.42509(11) 0.1003(2) 0.53621(14) 0.0291(4) Uani 1 1 d . . . . .
C11 C 0.44989(10) 0.5789(2) 0.76869(15) 0.0308(4) Uani 1 1 d . . . . .
C6 C 0.34044(12) 0.6253(2) 0.84175(14) 0.0329(4) Uani 1 1 d . . . . .
C7 C 0.27085(12) 0.6147(2) 0.84556(16) 0.0379(5) Uani 1 1 d . . . . .
C10 C 0.23329(13) 0.3946(3) 0.64211(17) 0.0417(6) Uani 1 1 d . . . . .
H1 H 0.4397(12) 0.268(2) 0.3655(17) 0.028(6) Uiso 1 1 d . . . . .
H2 H 0.4333(15) 0.008(3) 0.566(2) 0.043(8) Uiso 1 1 d . . . . .
H11A H 0.4661(15) 0.619(3) 0.816(2) 0.047(8) Uiso 1 1 d . . . . .
H11B H 0.4694(14) 0.487(3) 0.7720(19) 0.035(7) Uiso 1 1 d . . . . .
H6 H 0.3638(14) 0.680(3) 0.8823(19) 0.044(7) Uiso 1 1 d . . . . .
H11C H 0.4593(14) 0.610(3) 0.717(2) 0.048(8) Uiso 1 1 d . . . . .
H8 H 0.1943(15) 0.536(3) 0.7828(19) 0.037(7) Uiso 1 1 d . . . . .
H7 H 0.2491(15) 0.649(3) 0.892(2) 0.053(8) Uiso 1 1 d . . . . .
H10A H 0.2491(17) 0.307(4) 0.638(2) 0.063(10) Uiso 1 1 d . . . . .
H10B H 0.2358(18) 0.459(4) 0.584(3) 0.076(11) Uiso 1 1 d . . . . .
H10C H 0.1912(18) 0.406(4) 0.650(2) 0.063(10) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd01 Cl1 2.3087(5) . ?
Pd01 Cl2 2.2978(5) . ?
Pd01 N1 1.9980(14) . ?
Pd01 N2 2.0479(15) . ?
O1 C1 1.351(2) . ?
O1 C2 1.375(2) . ?
O2 C4 1.230(2) . ?
N1 C3 1.394(2) . ?
N1 C1 1.290(2) . ?
N2 C5 1.393(2) . ?
N2 C4 1.356(2) . ?
N3 C5 1.367(2) . ?
N3 C11 1.479(3) . ?
N3 C6 1.367(3) . ?
C5 C9 1.388(3) . ?
C9 C8 1.372(3) . ?
C9 C10 1.492(3) . ?
C4 C3 1.477(2) . ?
C3 C2 1.344(2) . ?
C1 H1 0.91(2) . ?
C8 C7 1.380(3) . ?
C8 H8 0.82(3) . ?
C2 H2 1.01(3) . ?
C11 H11A 0.86(3) . ?
C11 H11B 0.97(3) . ?
C11 H11C 0.85(3) . ?
C6 C7 1.371(3) . ?
C6 H6 0.92(3) . ?
C7 H7 0.88(3) . ?
C10 H10A 0.90(4) . ?
C10 H10B 1.06(4) . ?
C10 H10C 0.84(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
Cl2 Pd01 Cl1 93.537(17) . . ?
N1 Pd01 Cl1 91.26(4) . . ?
N1 Pd01 Cl2 175.14(4) . . ?
N1 Pd01 N2 80.33(6) . . ?
N2 Pd01 Cl1 171.59(4) . . ?
N2 Pd01 Cl2 94.88(4) . . ?
C1 O1 C2 106.10(15) . . ?
C3 N1 Pd01 113.33(11) . . ?
C1 N1 Pd01 139.74(13) . . ?
C1 N1 C3 106.90(15) . . ?
C5 N2 Pd01 126.71(12) . . ?
C4 N2 Pd01 116.81(12) . . ?
C4 N2 C5 116.21(15) . . ?
C5 N3 C11 119.56(16) . . ?
C5 N3 C6 120.20(17) . . ?
C6 N3 C11 120.24(17) . . ?
N3 C5 N2 119.71(16) . . ?
N3 C5 C9 120.10(16) . . ?
C9 C5 N2 120.18(16) . . ?
C5 C9 C10 119.50(18) . . ?
C8 C9 C5 119.14(18) . . ?
C8 C9 C10 121.36(19) . . ?
O2 C4 N2 126.29(17) . . ?
O2 C4 C3 122.70(16) . . ?
N2 C4 C3 110.96(15) . . ?
N1 C3 C4 117.65(15) . . ?
C2 C3 N1 107.70(16) . . ?
C2 C3 C4 134.49(17) . . ?
O1 C1 H1 119.2(15) . . ?
N1 C1 O1 111.62(17) . . ?
N1 C1 H1 129.1(15) . . ?
C9 C8 C7 120.7(2) . . ?
C9 C8 H8 121(2) . . ?
C7 C8 H8 119(2) . . ?
O1 C2 H2 115.7(18) . . ?
C3 C2 O1 107.67(17) . . ?
C3 C2 H2 135.9(18) . . ?
N3 C11 H11A 110.8(19) . . ?
N3 C11 H11B 107.7(16) . . ?
N3 C11 H11C 108(2) . . ?
H11A C11 H11B 103(3) . . ?
H11A C11 H11C 120(3) . . ?
H11B C11 H11C 106(3) . . ?
N3 C6 C7 120.5(2) . . ?
N3 C6 H6 119.4(17) . . ?
C7 C6 H6 119.9(17) . . ?
C8 C7 H7 120(2) . . ?
C6 C7 C8 119.3(2) . . ?
C6 C7 H7 120(2) . . ?
C9 C10 H10A 113(2) . . ?
C9 C10 H10B 103(2) . . ?
C9 C10 H10C 107(2) . . ?
H10A C10 H10B 118(3) . . ?
H10A C10 H10C 118(3) . . ?
H10B C10 H10C 96(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
Pd01 N1 C3 C4 5.1(2) . . . . ?
Pd01 N1 C3 C2 -178.85(13) . . . . ?
Pd01 N1 C1 O1 178.34(14) . . . . ?
Pd01 N2 C5 N3 -86.9(2) . . . . ?
Pd01 N2 C5 C9 92.48(19) . . . . ?
Pd01 N2 C4 O2 173.98(17) . . . . ?
Pd01 N2 C4 C3 -8.4(2) . . . . ?
O2 C4 C3 N1 179.83(18) . . . . ?
O2 C4 C3 C2 5.1(4) . . . . ?
N1 C3 C2 O1 0.1(2) . . . . ?
N2 C5 C9 C8 -179.26(18) . . . . ?
N2 C5 C9 C10 1.2(3) . . . . ?
N2 C4 C3 N1 2.2(2) . . . . ?
N2 C4 C3 C2 -172.5(2) . . . . ?
N3 C5 C9 C8 0.1(3) . . . . ?
N3 C5 C9 C10 -179.5(2) . . . . ?
N3 C6 C7 C8 0.8(4) . . . . ?
C5 N2 C4 O2 -11.6(3) . . . . ?
C5 N2 C4 C3 165.99(15) . . . . ?
C5 N3 C6 C7 -1.5(3) . . . . ?
C5 C9 C8 C7 -0.7(3) . . . . ?
C9 C8 C7 C6 0.3(4) . . . . ?
C4 N2 C5 N3 99.4(2) . . . . ?
C4 N2 C5 C9 -81.3(2) . . . . ?
C4 C3 C2 O1 175.16(19) . . . . ?
C3 N1 C1 O1 0.4(2) . . . . ?
C1 O1 C2 C3 0.1(2) . . . . ?
C1 N1 C3 C4 -176.31(17) . . . . ?
C1 N1 C3 C2 -0.3(2) . . . . ?
C2 O1 C1 N1 -0.3(2) . . . . ?
C11 N3 C5 N2 0.2(3) . . . . ?
C11 N3 C5 C9 -179.11(18) . . . . ?
C11 N3 C6 C7 178.7(2) . . . . ?
C6 N3 C5 N2 -179.64(17) . . . . ?
C6 N3 C5 C9 1.0(3) . . . . ?
C10 C9 C8 C7 178.8(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.413
_oxdiff_exptl_absorpt_empirical_full_min 0.732
####################################################################### 
# 
# 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_22MA060_ER-0474
_database_code_depnum_ccdc_archive 'CCDC 2394914'
loop_
_audit_author_name
_audit_author_address
'Lorraine Malaspina'
;University of Bern
Switzerland
;
_audit_update_record             
;
2024-10-30 deposited with the CCDC.	2024-12-18 downloaded from the CCDC.
;

_audit_creation_date             2022-05-16T17:04:23-00:00

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         'C19 H20 Cl2 N4 O Pd'
_chemical_formula_sum            'C19 H20 Cl2 N4 O Pd'
_chemical_formula_weight         497.69

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_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                   11.62997(6)
_cell_length_b                   14.78476(7)
_cell_length_c                   11.92053(6)
_cell_angle_alpha                90
_cell_angle_beta                 105.0469(5)
_cell_angle_gamma                90
_cell_volume                     1979.415(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    173.00(10)
_cell_measurement_reflns_used    34688
_cell_measurement_theta_min      2.999
_cell_measurement_theta_max      79.765

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.146
_exptl_crystal_size_mid          0.124
_exptl_crystal_size_min          0.07
_exptl_crystal_density_diffrn    1.67
_exptl_crystal_F_000             1000
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 1 0.0702
1 -1 -1 0.0628
1 -1 0 0.0657
0 -1 -1 0.0657
0 1 1 0.0657
-1 1 -1 0.0694
-1 -1 -1 0.0727
0 -1 0 0.0702
0 -1 1 0.0655
0 1 -1 0.0629
-1 -1 0 0.0672
1 1 0 0.0528
1 1 -1 0.0499
-1 -1 1 0.0388
0 0 -1 0.0451
1 0 0 0.0537
1 0 -1 0.0351
-1 0 1 0.0351
-1 0 0 0.0551
0 0 1 0.0676
2 9 1 0.045

loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.9996 0.0003 0.9994 0.0066 -0.0098 -0.2147
1.0007 -0.9981 -1.0009 0.1941 -0.0189 0.0026
1.0006 -0.9991 -0.0011 0.1323 0.0267 -0.107
0.001 -0.9993 -1.0005 0.1258 0.0366 0.1078
-0.001 0.9993 1.0005 -0.1258 -0.0366 -0.1078
-1.0005 1 -0.9986 -0.0706 -0.0724 0.2165
-0.9988 -1.0005 -1.0002 0.0574 0.0921 0.2129
0.0008 -1.0003 -0.0008 0.064 0.0822 -0.0018
0.0007 -1.0012 0.9989 0.0023 0.1279 -0.1114
-0.0007 1.0012 -0.9989 -0.0023 -0.1279 0.1114
-0.9989 -1.0015 -0.0005 -0.0043 0.1377 0.1033
0.9989 1.0015 0.0005 0.0043 -0.1377 -0.1033
0.9991 1.0024 -0.9992 0.0661 -0.1834 0.0062
-0.9991 -1.0024 0.9992 -0.0661 0.1834 -0.0062
0.0001 0.0009 -0.9997 0.0617 -0.0457 0.1096
0.9998 0.0012 -0.0003 0.0683 -0.0555 -0.1051
0.9999 0.0021 -1 0.1301 -0.1011 0.0044
-0.9999 -0.0021 1 -0.1301 0.1011 -0.0044
-0.9998 -0.0012 0.0003 -0.0683 0.0555 0.1051
-0.0001 -0.0009 0.9997 -0.0617 0.0457 -0.1096
1.8042 9.001 1.3994 -0.5382 -0.7768 -0.327


#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    10.184
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
        Empirical absorption correction using spherical harmonics,
        implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.51465
_exptl_absorpt_correction_T_max  1
_shelx_estimated_absorpt_T_min   0.318
_shelx_estimated_absorpt_T_max   0.536
_oxdiff_exptl_absorpt_empirical_details 
;
        Empirical correction (ABSPACK) includes:
        - Absorption correction using spherical harmonics
        - Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.319
_oxdiff_exptl_absorpt_empirical_full_min 0.703

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_ambient_temperature      173.00(10)
_diffrn_ambient_environment      N~2~
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_type            HyPix
_diffrn_detector_area_resol_mean 10
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_ub_11      0.0683971
_diffrn_orient_matrix_ub_12      -0.0638919
_diffrn_orient_matrix_ub_13      -0.0618171
_diffrn_orient_matrix_ub_21      -0.055381
_diffrn_orient_matrix_ub_22      -0.0822884
_diffrn_orient_matrix_ub_23      0.0455843
_diffrn_orient_matrix_ub_31      -0.105212
_diffrn_orient_matrix_ub_32      0.0018057
_diffrn_orient_matrix_ub_33      -0.1096329
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_number            39723
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         4.733
_diffrn_reflns_theta_max         73.73
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 1
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 1
_reflns_Friedel_coverage         0
_reflns_number_total             4006
_reflns_number_gt                3994
_reflns_threshold_expression     'I > 2σ(I)'
_diffrn_measurement_details      
;
        List of Runs (angles in degrees, time in seconds):
  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -77.00 -19.00   0.50    0.24    --  -23.00 137.00 -96.00  116
  2  ω    -74.00 -16.00   0.50    0.24    --  -23.00 132.00  86.00  116
  3  ω    -70.00 -12.00   0.50    0.24    --  -23.00 125.00 -90.00  116
  4  ω    -21.00   5.00   0.50    0.24    --  -23.00 -88.00 -25.19   52
  5  ω    -70.00 -12.00   0.50    0.24    --  -23.00 125.00 120.00  116
  6  ω    -95.00  -6.00   0.50    0.24    --  -23.00 -61.00   0.00  178
  7  ω    -95.00   0.00   0.50    0.24    --  -23.00 -77.00 150.00  190
  8  ω    -25.00  40.00   0.50    0.24    --   47.92 -38.00 -90.00  130
  9  ω    -25.00  40.00   0.50    0.24    --   47.92 -38.00   0.00  130
 10  ω    -26.00  23.00   0.50    0.24    --   47.92 -19.00-150.00   98
 11  ω    -25.00  40.00   0.50    0.24    --   47.92 -38.00-180.00  130
 12  ω    -26.00  23.00   0.50    0.24    --   47.92 -19.00  30.00   98
 13  ω    -23.00  63.00   0.50    0.24    --   47.92 -57.00 -30.00  172
 14  ω     42.00  68.00   0.50    0.80    --  113.25 -61.00  60.00   52
 15  ω     42.00  68.00   0.50    0.80    --  113.25 -61.00 120.00   52
 16  ω     42.00 106.00   0.50    0.80    --  113.25 -94.00 -90.00  128
 17  ω     97.00 177.00   0.50    0.80    --  113.25  61.00   0.00  160
 18  ω    101.00 177.00   0.50    0.80    --  113.25  30.00 150.00  152
 19  ω     42.00 102.00   0.50    0.80    --  113.25 -77.00  30.00  120
 20  ω    100.00 177.00   0.50    0.80    --  113.25  15.00 -90.00  154
 21  ω     42.00 106.00   0.50    0.80    --  113.25 -94.00   0.00  128
 22  ω     42.00 106.00   0.50    0.80    --  113.25 -94.00-180.00  128
 23  ω     42.00 106.00   0.50    0.80    --  113.25 -94.00  30.00  128
 24  ω    101.00 177.00   0.50    0.80    --  113.25  45.00-150.00  152
 25  ω    101.00 177.00   0.50    0.80    --  113.25  30.00 -30.00  152
 26  ω     42.00 106.00   0.50    0.80    --  113.25 -94.00 -30.00  128
 27  ω     42.00 106.00   0.50    0.80    --  113.25 -94.00-150.00  128
 28  ω     42.00 106.00   0.50    0.80    --  113.25 -94.00 -60.00  128
 29  ω    100.00 177.00   0.50    0.80    --  113.25  15.00  90.00  154
 30  ω     42.00 102.00   0.50    0.80    --  113.25 -77.00 120.00  120
 31  ω     42.00  68.00   0.50    0.80    --  113.25 -61.00-120.00   52
 32  ω     42.00 106.00   0.50    0.80    --  113.25 -94.00 120.00  128
 33  ω     42.00 106.00   0.50    0.80    --  113.25 -94.00-120.00  128
 34  ω    101.00 177.00   0.50    0.80    --  113.25  45.00-180.00  152
 35  ω    101.00 177.00   0.50    0.80    --  113.25  45.00  30.00  152
 36  ω     42.00 106.00   0.50    0.80    --  113.25 -94.00  90.00  128
 37  ω     42.00  68.00   0.50    0.80    --  113.25 -61.00  30.00   52
 38  ω     42.00 102.00   0.50    0.80    --  113.25 -77.00 150.00  120
 39  ω     42.00 106.00   0.50    0.80    --  113.25 -94.00  60.00  128
 40  ω     42.00  68.00   0.50    0.80    --  113.25 -61.00-150.00   52
 41  ω     42.00 102.00   0.50    0.80    --  113.25 -77.00-180.00  120
 42  ω     97.00 177.00   0.50    0.80    --  113.25  61.00 -30.00  160
 43  ω    101.00 177.00   0.50    0.80    --  113.25  45.00 -90.00  152
 44  ω     42.00 109.00   0.50    0.80    --  113.25-114.00  35.04  134
 45  ω     25.00 121.00   0.50    0.24    --   47.92  77.00   0.00  192
 46  ω     25.00 121.00   0.50    0.24    --   47.92  77.00-180.00  192
 47  ω     25.00 121.00   0.50    0.24    --   47.92  77.00  90.00  192
 48  ω     25.00 121.00   0.50    0.24    --   47.92  77.00 -60.00  192
 49  ω     25.00 121.00   0.50    0.24    --   47.92  77.00 -90.00  192
;

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     dual
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_shelx_SHELXL_version_number     2018/3
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0234P)²+2.2183P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         4006
_refine_ls_number_parameters     267
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.0238
_refine_ls_R_factor_gt           0.0237
_refine_ls_wR_factor_ref         0.0615
_refine_ls_wR_factor_gt          0.0615
_refine_ls_goodness_of_fit_ref   1.17
_refine_ls_restrained_S_all      1.165
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.434
_refine_diff_density_min         -0.514
_refine_diff_density_rms         0.06
_olex2_refinement_description    
;
        1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
        2. Rigid bond restraints
 C5A, C1, C2, C3, N1A, C4, C6, C7
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
        3. Uiso/Uaniso restraints and constraints
Uanis(N1A) \\sim Ueq, Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for
        terminal atoms of 0.02
Uanis(C5A) \\sim Ueq, Uanis(N1) \\sim Ueq: with sigma of 0.01 and sigma for
        terminal atoms of 0.02
        4. Others
 Sof(H1BD)=Sof(H1BE)=Sof(H1BF)=Sof(H7BD)=Sof(H7BE)=Sof(H7BF)=Sof(H4B)=Sof(H2B)=
 Sof(C5A)=Sof(N1A)=1-FVAR(1)
 Sof(N1)=Sof(C5)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=
 Sof(H4A)=Sof(H2A)=FVAR(1)
        5.a Me refined with riding coordinates:
 C1(H1BD,H1BE,H1BF), C7(H7BD,H7BE,H7BF)
        5.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C10(H10), C17(H17), C13(H13), C4(H4A), C4(H4B), C2(H2A), C2(H2B),
 C15(H15), C3(H3)
        5.c Idealised Me refined as rotating group:
 C1(H1AA,H1AB,H1AC), C7(H7AA,H7AB,H7AC), C19(H19A,H19B,H19C), C18(H18A,H18B,
 H18C)
;

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.018 '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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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 0.21873(2) 0.36634(2) 0.29526(2) 0.02397(6) Uani 1 1 d . . . . .
Cl2 Cl 0.10222(5) 0.27270(4) 0.37300(5) 0.03536(14) Uani 1 1 d . . . . .
Cl1 Cl 0.08778(6) 0.36133(5) 0.11594(5) 0.03972(15) Uani 1 1 d . . . . .
O1 O 0.54170(14) 0.46938(12) 0.28166(14) 0.0312(4) Uani 1 1 d . . . . .
N3 N 0.35238(17) 0.38039(13) 0.44337(16) 0.0247(4) Uani 1 1 d . . . . .
N4 N 0.37944(17) 0.35054(13) 0.55488(16) 0.0253(4) Uani 1 1 d . . . . .
N2 N 0.34014(17) 0.43785(14) 0.23402(16) 0.0277(4) Uani 1 1 d . . . . .
N1 N 0.2555(13) 0.5389(9) 0.0792(8) 0.0299(17) Uani 0.709(19) 1 d . U P A 1
C9 C 0.4567(2) 0.40098(16) 0.4216(2) 0.0262(4) Uani 1 1 d . . . . .
C12 C 0.2928(2) 0.33975(17) 0.6202(2) 0.0283(5) Uani 1 1 d . . . . .
C5 C 0.377(2) 0.4197(18) 0.0474(15) 0.030(2) Uani 0.709(19) 1 d . U P A 1
C11 C 0.4988(2) 0.35328(16) 0.6011(2) 0.0292(5) Uani 1 1 d . . . . .
H11 H 0.539426 0.336067 0.677962 0.035 Uiso 1 1 calc R U . . .
C10 C 0.5508(2) 0.38511(17) 0.5182(2) 0.0288(5) Uani 1 1 d . . . . .
H10 H 0.633214 0.394297 0.525204 0.035 Uiso 1 1 calc R U . . .
C8 C 0.4526(2) 0.43859(16) 0.30523(19) 0.0263(5) Uani 1 1 d . . . . .
C6 C 0.3245(2) 0.46671(16) 0.12052(19) 0.0269(4) Uani 1 1 d . U . . .
C17 C 0.3118(2) 0.27247(18) 0.7033(2) 0.0328(5) Uani 1 1 d . . . . .
H17 H 0.376271 0.231443 0.711415 0.039 Uiso 1 1 calc R U . . .
C13 C 0.1997(2) 0.4005(2) 0.6056(2) 0.0358(6) Uani 1 1 d . . . . .
H13 H 0.189485 0.446664 0.548515 0.043 Uiso 1 1 calc R U . . .
C1 C 0.1961(3) 0.5899(2) 0.1610(3) 0.0420(6) Uani 1 1 d . U . . .
H1AA H 0.256911 0.608756 0.230549 0.063 Uiso 0.709(19) 1 calc R U P A 1
H1AB H 0.138516 0.550101 0.183606 0.063 Uiso 0.709(19) 1 calc R U P A 1
H1AC H 0.154958 0.643313 0.121305 0.063 Uiso 0.709(19) 1 calc R U P A 1
H1BD H 0.219101 0.562594 0.238592 0.063 Uiso 0.291(19) 1 calc R U P A 2
H1BE H 0.218312 0.653961 0.166413 0.063 Uiso 0.291(19) 1 calc R U P A 2
H1BF H 0.109858 0.584215 0.129006 0.063 Uiso 0.291(19) 1 calc R U P A 2
C7 C 0.4453(3) 0.3367(2) 0.0818(3) 0.0428(6) Uani 1 1 d . U . . .
H7AA H 0.39996 0.295165 0.118122 0.064 Uiso 0.709(19) 1 calc R U P A 1
H7AB H 0.521155 0.351324 0.137286 0.064 Uiso 0.709(19) 1 calc R U P A 1
H7AC H 0.46055 0.30794 0.012998 0.064 Uiso 0.709(19) 1 calc R U P A 1
H7BD H 0.44559 0.326307 0.16307 0.064 Uiso 0.291(19) 1 calc R U P A 2
H7BE H 0.407821 0.285122 0.03456 0.064 Uiso 0.291(19) 1 calc R U P A 2
H7BF H 0.527301 0.343427 0.075852 0.064 Uiso 0.291(19) 1 calc R U P A 2
C16 C 0.2348(3) 0.2657(2) 0.7753(2) 0.0417(7) Uani 1 1 d . . . . .
C4 C 0.3599(3) 0.4532(2) -0.0670(2) 0.0433(5) Uani 1 1 d . U . . .
H4A H 0.396749 0.423278 -0.119041 0.052 Uiso 0.709(19) 1 calc R U P A 1
H4B H 0.396852 0.423028 -0.11877 0.052 Uiso 0.291(19) 1 calc R U P A 2
C2 C 0.2375(3) 0.5713(2) -0.0288(2) 0.0454(6) Uani 1 1 d . U . . .
H2A H 0.18869 0.622822 -0.053195 0.054 Uiso 0.709(19) 1 calc R U P A 1
H2B H 0.186801 0.62069 -0.059234 0.054 Uiso 0.291(19) 1 calc R U P A 2
C14 C 0.1213(3) 0.3932(2) 0.6753(3) 0.0472(7) Uani 1 1 d . . . . .
C15 C 0.1407(3) 0.3257(2) 0.7594(3) 0.0494(8) Uani 1 1 d . . . . .
H15 H 0.087583 0.320667 0.807605 0.059 Uiso 1 1 calc R U . . .
C3 C 0.2915(3) 0.5280(2) -0.1036(2) 0.0493(6) Uani 1 1 d . U . . .
H3 H 0.281254 0.550065 -0.180428 0.059 Uiso 1 1 calc R U . . .
C19 C 0.2568(3) 0.1946(3) 0.8691(3) 0.0588(10) Uani 1 1 d . . . . .
H19A H 0.205701 0.142139 0.841761 0.088 Uiso 1 1 calc R U . . .
H19B H 0.238607 0.219524 0.938695 0.088 Uiso 1 1 calc R U . . .
H19C H 0.340493 0.175895 0.887819 0.088 Uiso 1 1 calc R U . . .
C18 C 0.0190(3) 0.4594(3) 0.6614(4) 0.0728(12) Uani 1 1 d . . . . .
H18A H 0.029134 0.508967 0.610258 0.109 Uiso 1 1 calc R U . . .
H18B H 0.01811 0.483789 0.73762 0.109 Uiso 1 1 calc R U . . .
H18C H -0.056333 0.428198 0.627387 0.109 Uiso 1 1 calc R U . . .
C5A C 0.251(4) 0.548(3) 0.093(3) 0.033(3) Uani 0.291(19) 1 d . U P A 2
N1A N 0.375(5) 0.423(4) 0.038(3) 0.031(3) Uani 0.291(19) 1 d . U P A 2



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 Cl2 2.2941(6) . ?
Pd1 Cl1 2.2812(6) . ?
Pd1 N3 2.0375(19) . ?
Pd1 N2 2.0444(19) . ?
O1 C8 1.230(3) . ?
N3 N4 1.358(3) . ?
N3 C9 1.339(3) . ?
N4 C12 1.434(3) . ?
N4 C11 1.354(3) . ?
N2 C8 1.362(3) . ?
N2 C6 1.385(3) . ?
N1 C6 1.349(10) . ?
N1 C1 1.532(7) . ?
N1 C2 1.338(9) . ?
C9 C10 1.387(3) . ?
C9 C8 1.484(3) . ?
C12 C17 1.381(4) . ?
C12 C13 1.382(4) . ?
C5 C6 1.37(2) . ?
C5 C7 1.46(2) . ?
C5 C4 1.416(16) . ?
C11 H11 0.95 . ?
C11 C10 1.370(3) . ?
C10 H10 0.95 . ?
C6 C5A 1.46(3) . ?
C6 N1A 1.42(5) . ?
C17 H17 0.95 . ?
C17 C16 1.395(4) . ?
C13 H13 0.95 . ?
C13 C14 1.388(4) . ?
C1 H1AA 0.98 . ?
C1 H1AB 0.98 . ?
C1 H1AC 0.98 . ?
C1 H1BD 0.98 . ?
C1 H1BE 0.98 . ?
C1 H1BF 0.98 . ?
C1 C5A 1.31(3) . ?
C7 H7AA 0.98 . ?
C7 H7AB 0.98 . ?
C7 H7AC 0.98 . ?
C7 H7BD 0.98 . ?
C7 H7BE 0.98 . ?
C7 H7BF 0.98 . ?
C7 N1A 1.54(5) . ?
C16 C15 1.383(5) . ?
C16 C19 1.508(4) . ?
C4 H4A 0.95 . ?
C4 H4B 0.95 . ?
C4 C3 1.366(5) . ?
C4 N1A 1.29(4) . ?
C2 H2A 0.95 . ?
C2 H2B 0.95 . ?
C2 C3 1.373(5) . ?
C2 C5A 1.46(3) . ?
C14 C15 1.391(5) . ?
C14 C18 1.516(5) . ?
C15 H15 0.95 . ?
C3 H3 0.95 . ?
C19 H19A 0.98 . ?
C19 H19B 0.98 . ?
C19 H19C 0.98 . ?
C18 H18A 0.98 . ?
C18 H18B 0.98 . ?
C18 H18C 0.98 . ?

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
Cl1 Pd1 Cl2 92.19(2) . . ?
N3 Pd1 Cl2 96.27(6) . . ?
N3 Pd1 Cl1 171.42(6) . . ?
N3 Pd1 N2 79.31(8) . . ?
N2 Pd1 Cl2 172.48(6) . . ?
N2 Pd1 Cl1 92.13(6) . . ?
N4 N3 Pd1 138.24(15) . . ?
C9 N3 Pd1 112.39(15) . . ?
C9 N3 N4 105.78(18) . . ?
N3 N4 C12 123.44(19) . . ?
C11 N4 N3 109.96(19) . . ?
C11 N4 C12 124.94(19) . . ?
C8 N2 Pd1 114.96(15) . . ?
C8 N2 C6 117.92(19) . . ?
C6 N2 Pd1 125.46(15) . . ?
C6 N1 C1 118.7(6) . . ?
C2 N1 C6 124.4(5) . . ?
C2 N1 C1 116.9(7) . . ?
N3 C9 C10 111.1(2) . . ?
N3 C9 C8 117.1(2) . . ?
C10 C9 C8 131.7(2) . . ?
C17 C12 N4 117.8(2) . . ?
C17 C12 C13 122.2(2) . . ?
C13 C12 N4 119.8(2) . . ?
C6 C5 C7 123.0(12) . . ?
C6 C5 C4 117.4(15) . . ?
C4 C5 C7 119.5(15) . . ?
N4 C11 H11 125.8 . . ?
N4 C11 C10 108.3(2) . . ?
C10 C11 H11 125.8 . . ?
C9 C10 H10 127.6 . . ?
C11 C10 C9 104.8(2) . . ?
C11 C10 H10 127.6 . . ?
O1 C8 N2 126.2(2) . . ?
O1 C8 C9 121.9(2) . . ?
N2 C8 C9 111.86(19) . . ?
N2 C6 C5A 113.1(12) . . ?
N2 C6 N1A 124.4(17) . . ?
N1 C6 N2 121.1(3) . . ?
N1 C6 C5 119.2(8) . . ?
C5 C6 N2 119.7(8) . . ?
N1A C6 C5A 122(2) . . ?
C12 C17 H17 120.5 . . ?
C12 C17 C16 119.0(3) . . ?
C16 C17 H17 120.5 . . ?
C12 C13 H13 120.4 . . ?
C12 C13 C14 119.3(3) . . ?
C14 C13 H13 120.4 . . ?
N1 C1 H1AA 109.5 . . ?
N1 C1 H1AB 109.5 . . ?
N1 C1 H1AC 109.5 . . ?
H1AA C1 H1AB 109.5 . . ?
H1AA C1 H1AC 109.5 . . ?
H1AB C1 H1AC 109.5 . . ?
H1BD C1 H1BE 109.5 . . ?
H1BD C1 H1BF 109.5 . . ?
H1BE C1 H1BF 109.5 . . ?
C5A C1 H1BD 109.5 . . ?
C5A C1 H1BE 109.5 . . ?
C5A C1 H1BF 109.5 . . ?
C5 C7 H7AA 109.5 . . ?
C5 C7 H7AB 109.5 . . ?
C5 C7 H7AC 109.5 . . ?
H7AA C7 H7AB 109.5 . . ?
H7AA C7 H7AC 109.5 . . ?
H7AB C7 H7AC 109.5 . . ?
H7BD C7 H7BE 109.5 . . ?
H7BD C7 H7BF 109.5 . . ?
H7BE C7 H7BF 109.5 . . ?
N1A C7 H7BD 109.5 . . ?
N1A C7 H7BE 109.5 . . ?
N1A C7 H7BF 109.5 . . ?
C17 C16 C19 119.6(3) . . ?
C15 C16 C17 118.7(3) . . ?
C15 C16 C19 121.7(3) . . ?
C5 C4 H4A 119.5 . . ?
C3 C4 C5 120.9(10) . . ?
C3 C4 H4A 119.5 . . ?
C3 C4 H4B 119.8 . . ?
N1A C4 H4B 119.8 . . ?
N1A C4 C3 120(2) . . ?
N1 C2 H2A 120.8 . . ?
N1 C2 C3 118.3(4) . . ?
C3 C2 H2A 120.8 . . ?
C3 C2 H2B 117 . . ?
C3 C2 C5A 126.0(13) . . ?
C5A C2 H2B 117 . . ?
C13 C14 C15 118.5(3) . . ?
C13 C14 C18 120.2(3) . . ?
C15 C14 C18 121.2(3) . . ?
C16 C15 C14 122.3(3) . . ?
C16 C15 H15 118.9 . . ?
C14 C15 H15 118.9 . . ?
C4 C3 C2 119.7(3) . . ?
C4 C3 H3 120.1 . . ?
C2 C3 H3 120.1 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C14 C18 H18A 109.5 . . ?
C14 C18 H18B 109.5 . . ?
C14 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C1 C5A C6 127(3) . . ?
C1 C5A C2 124(3) . . ?
C2 C5A C6 108.6(19) . . ?
C6 N1A C7 115(3) . . ?
C4 N1A C6 123(4) . . ?
C4 N1A C7 123(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
Pd1 N3 N4 C12 -38.1(3) . . . . ?
Pd1 N3 N4 C11 155.96(19) . . . . ?
Pd1 N3 C9 C10 -162.98(16) . . . . ?
Pd1 N3 C9 C8 19.2(3) . . . . ?
Pd1 N2 C8 O1 172.4(2) . . . . ?
Pd1 N2 C8 C9 -10.5(2) . . . . ?
Pd1 N2 C6 N1 76.8(9) . . . . ?
Pd1 N2 C6 C5 -101.2(15) . . . . ?
Pd1 N2 C6 C5A 79(2) . . . . ?
Pd1 N2 C6 N1A -101(3) . . . . ?
N3 N4 C12 C17 149.0(2) . . . . ?
N3 N4 C12 C13 -36.3(3) . . . . ?
N3 N4 C11 C10 -0.3(3) . . . . ?
N3 C9 C10 C11 0.1(3) . . . . ?
N3 C9 C8 O1 171.3(2) . . . . ?
N3 C9 C8 N2 -5.9(3) . . . . ?
N4 N3 C9 C10 -0.3(3) . . . . ?
N4 N3 C9 C8 -178.09(19) . . . . ?
N4 C12 C17 C16 174.3(2) . . . . ?
N4 C12 C13 C14 -175.4(2) . . . . ?
N4 C11 C10 C9 0.1(3) . . . . ?
N2 C6 C5A C1 -5(6) . . . . ?
N2 C6 C5A C2 -179(2) . . . . ?
N2 C6 N1A C7 3(5) . . . . ?
N2 C6 N1A C4 -179(3) . . . . ?
N1 C2 C3 C4 0.9(10) . . . . ?
C9 N3 N4 C12 166.3(2) . . . . ?
C9 N3 N4 C11 0.3(2) . . . . ?
C12 N4 C11 C10 -166.0(2) . . . . ?
C12 C17 C16 C15 1.1(4) . . . . ?
C12 C17 C16 C19 -177.9(2) . . . . ?
C12 C13 C14 C15 1.2(4) . . . . ?
C12 C13 C14 C18 179.6(3) . . . . ?
C5 C4 C3 C2 -0.4(15) . . . . ?
C11 N4 C12 C17 -47.1(3) . . . . ?
C11 N4 C12 C13 127.5(3) . . . . ?
C10 C9 C8 O1 -6.0(4) . . . . ?
C10 C9 C8 N2 176.8(2) . . . . ?
C8 N2 C6 N1 -118.7(9) . . . . ?
C8 N2 C6 C5 63.3(15) . . . . ?
C8 N2 C6 C5A -116(2) . . . . ?
C8 N2 C6 N1A 63(3) . . . . ?
C8 C9 C10 C11 177.5(2) . . . . ?
C6 N2 C8 O1 6.3(4) . . . . ?
C6 N2 C8 C9 -176.7(2) . . . . ?
C6 N1 C2 C3 0.7(19) . . . . ?
C6 C5 C4 C3 -2(3) . . . . ?
C17 C12 C13 C14 -1.0(4) . . . . ?
C17 C16 C15 C14 -0.8(4) . . . . ?
C13 C12 C17 C16 -0.2(4) . . . . ?
C13 C14 C15 C16 -0.4(5) . . . . ?
C1 N1 C6 N2 1.1(16) . . . . ?
C1 N1 C6 C5 179.1(16) . . . . ?
C1 N1 C2 C3 178.8(8) . . . . ?
C7 C5 C6 N2 3(3) . . . . ?
C7 C5 C6 N1 -175.1(17) . . . . ?
C7 C5 C4 C3 176.7(13) . . . . ?
C4 C5 C6 N2 -178.7(13) . . . . ?
C4 C5 C6 N1 3(3) . . . . ?
C2 N1 C6 N2 179.1(10) . . . . ?
C2 N1 C6 C5 -3(2) . . . . ?
C3 C4 N1A C6 -2(6) . . . . ?
C3 C4 N1A C7 177(3) . . . . ?
C3 C2 C5A C6 -4(5) . . . . ?
C3 C2 C5A C1 -179(3) . . . . ?
C19 C16 C15 C14 178.2(3) . . . . ?
C18 C14 C15 C16 -178.7(3) . . . . ?
C5A C6 N1A C7 -178(3) . . . . ?
C5A C6 N1A C4 1(6) . . . . ?
C5A C2 C3 C4 4(3) . . . . ?
N1A C6 C5A C1 176(4) . . . . ?
N1A C6 C5A C2 2(5) . . . . ?
N1A C4 C3 C2 0(3) . . . . ?


#----------------------------------------------------------------------------#
#                       SHELX RES FILE                                       #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                       SHELX HKL FILE                                       #
#----------------------------------------------------------------------------#


# END of CIF
####################################################################### 
# 
# 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_23MA063_MA-055
_database_code_depnum_ccdc_archive 'CCDC 2394915'
loop_
_audit_author_name
_audit_author_address
'Lorraine Malaspina'
;University of Bern
Switzerland
;
_audit_update_record             
;
2024-12-04 deposited with the CCDC.	2024-12-18 downloaded from the CCDC.
;

_audit_creation_date             2023-10-11T15:12:08-00:00

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         'C14 H18 Cl2 N4 O Pd'
_chemical_formula_sum            'C14 H18 Cl2 N4 O Pd'
_chemical_formula_weight         435.62
_chemical_absolute_configuration unk

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_Int_Tables_number      19
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   8.91557(12)
_cell_length_b                   10.26115(13)
_cell_length_c                   18.9836(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1736.70(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    173.00(10)
_cell_measurement_reflns_used    54838
_cell_measurement_theta_min      2.238
_cell_measurement_theta_max      33.115

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       needle
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.338
_exptl_crystal_size_mid          0.117
_exptl_crystal_size_min          0.069
_exptl_crystal_density_diffrn    1.666
_exptl_crystal_F_000             872
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 1 0.1497
-1 0 -1 0.1575
1 1 1 0.1281
0 1 0 0.0265
-1 1 -1 0.1226
1 1 0 0.1334
-1 -1 0 0.1479
0 -1 1 0.0493
0 1 -1 0.0212
-1 -1 1 0.1436
1 0 0 0.1683
-1 0 0 0.17
-1 0 1 0.1737
1 0 -1 0.1616
0 0 1 0.0745
0 0 -1 0.0421
1 -1 -1 0.129
-1 1 1 0.1451
1 -1 0 0.1334
-1 1 0 0.1377
0 -1 -1 0.025
0 1 1 0.046

loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.9993 -0.0002 0.9989 -0.0289 0.0085 -0.0825
-0.9993 0.0002 -0.9989 0.0289 -0.0085 0.0825
0.9994 0.999 0.9998 -0.0939 0.0112 -0.0594
0.0002 0.9992 0.0009 -0.065 0.0026 0.0231
-0.9991 0.9994 -0.998 -0.0361 -0.0059 0.1056
0.9994 0.9991 0.0008 -0.091 -0.024 -0.0472
-0.9994 -0.9991 -0.0008 0.091 0.024 0.0472
-0.0001 -0.9993 0.9981 0.0621 0.0325 -0.0353
0.0001 0.9993 -0.9981 -0.0621 -0.0325 0.0353
-0.9994 -0.9993 0.9982 0.0881 0.0591 0.0349
0.9992 -0.0001 -0.0001 -0.026 -0.0266 -0.0703
-0.9992 0.0001 0.0001 0.026 0.0266 0.0703
-0.9992 -0.0001 0.9991 0.0231 0.0618 0.0581
0.9992 0.0001 -0.9991 -0.0231 -0.0618 -0.0581
0 -0.0002 0.999 -0.0029 0.0351 -0.0122
0 0.0002 -0.999 0.0029 -0.0351 0.0122
0.9991 -0.9991 -1 0.0419 -0.0644 -0.0812
-0.9991 0.9991 1 -0.0419 0.0644 0.0812
0.9991 -0.9992 -0.001 0.039 -0.0293 -0.0934
-0.9991 0.9992 0.001 -0.039 0.0293 0.0934
-0.0002 -0.999 -0.9999 0.0679 -0.0378 -0.0109
0.0002 0.999 0.9999 -0.0679 0.0378 0.0109


#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.382
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
        CrysAlisPro 1.171.42.89a (Rigaku Oxford Diffraction, 2023)
        Numerical absorption correction based on gaussian integration over
        a multifaceted crystal model
        Empirical absorption correction using spherical harmonics,
        implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.561
_exptl_absorpt_correction_T_max  1
_shelx_estimated_absorpt_T_min   0.652
_shelx_estimated_absorpt_T_max   0.911
_oxdiff_exptl_absorpt_empirical_details 
;
        Empirical correction (ABSPACK) includes:
        - Absorption correction using spherical harmonics
        - Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.246
_oxdiff_exptl_absorpt_empirical_full_min 0.884

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_diffrn_ambient_temperature      173.00(10)
_diffrn_ambient_environment      N~2~
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_detector_area_resol_mean 10
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_ub_11      -0.0260363
_diffrn_orient_matrix_ub_12      -0.0650673
_diffrn_orient_matrix_ub_13      -0.0029165
_diffrn_orient_matrix_ub_21      -0.0266346
_diffrn_orient_matrix_ub_22      0.0026213
_diffrn_orient_matrix_ub_23      0.0351803
_diffrn_orient_matrix_ub_31      -0.0703291
_diffrn_orient_matrix_ub_32      0.023157
_diffrn_orient_matrix_ub_33      -0.012222
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix-Arc 100'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_av_unetI/netI     0.0498
_diffrn_reflns_number            105258
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.146
_diffrn_reflns_theta_max         30.504
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 1
_reflns_Friedel_fraction_full    1
_reflns_Friedel_fraction_max     1
_reflns_Friedel_coverage         0.767
_reflns_number_total             5302
_reflns_number_gt                4819
_reflns_threshold_expression     'I > 2σ(I)'
_diffrn_measurement_details      
;
        List of Runs (angles in degrees, time in seconds):
  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
        --------------------------------------------------------------------------
  1  ω    -28.00  21.00   0.50    0.30    --   13.07  99.00 148.00   98
  2  ω    -18.00  54.00   0.50    0.30    --   13.07 -99.00  42.00  144
  3  ω    -55.00  21.00   0.50    0.30    --  -13.54  99.00 148.00  152
  4  ω    -19.00  29.00   0.50    0.30    --  -13.54 -99.00  42.00   96
  5  ω     -8.00  90.00   0.50    0.30    --   13.07  57.00  60.00  196
  6  ω     -8.00  90.00   0.50    0.30    --   13.07  57.00-150.00  196
  7  ω     -8.00  90.00   0.50    0.30    --   13.07  57.00 -30.00  196
  8  ω    -25.00  67.00   0.50    0.30    --  -13.54  19.00 -90.00  184
  9  ω    -80.00 -21.00   0.50    0.30    --  -13.54 139.00   8.90  118
 10  ω    -80.00 -21.00   0.50    0.30    --  -13.54 139.00-153.00  118
 11  ω    -25.00  67.00   0.50    0.30    --  -13.54  19.00  90.00  184
 12  ω    -25.00  67.00   0.50    0.30    --  -13.54  19.00   0.00  184
 13  ω    -68.00  28.00   0.50    0.30    --   13.07 -19.00 150.00  192
 14  ω    -25.00  67.00   0.50    0.30    --  -13.54  19.00 -60.00  184
 15  ω    -80.00 -21.00   0.50    0.30    --  -13.54 139.00 113.36  118
 16  ω    -74.00 -17.00   0.50    0.30    --  -13.54 130.00 -27.00  114
 17  ω    -87.00 -42.00   0.50    0.30    --  -13.54-178.00  60.00   90
 18  ω    -80.00 -21.00   0.50    0.30    --  -13.54 139.00  70.78  118
 19  ω    -78.00 -20.00   0.50    0.30    --  -13.54 136.00 169.69  116
 20  ω    -80.00 -21.00   0.50    0.30    --  -13.54 139.00 -86.99  118
 21  ω    -19.00  29.00   0.50    0.30    --  -13.54 -99.00  60.00   96
 22  ω    -79.00 -21.00   0.50    0.30    --  -13.54 138.00  97.18  116
 23  ω     -8.00  19.00   0.50    0.30    --   13.07  57.00-180.00   54
 24  ω    -80.00 -21.00   0.50    0.30    --  -13.54 139.00-129.87  118
 25  ω    -80.00 -21.00   0.50    0.30    --  -13.54 139.00  35.05  118
;

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'

#----------------------------------------------------------------------------#
#                   TWINNING                                                 #
#----------------------------------------------------------------------------#

loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.51(7)
2 0.49(7)


#----------------------------------------------------------------------------#
#                   SQUEEZE                                                  #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     dual
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_shelx_SHELXL_version_number     2018/3
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0300P)²+1.5001P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         5302
_refine_ls_number_parameters     328
_refine_ls_number_restraints     226
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.033
_refine_ls_wR_factor_ref         0.0781
_refine_ls_wR_factor_gt          0.0763
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_restrained_S_all      1.125
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.49(7)
_refine_diff_density_max         1.154
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.071

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#

_olex2_refinement_description    
;
        1. Twinned data refinement
 Scales: 0.51(7)
 0.49(7)
        2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
        3. Shared sites
        {C2, N1A}
        {C2A, N1}
        4. Restrained distances
 N1-C7 \\sim N1A-C7A
 with sigma of 0.002
 C2A-C6A \\sim C6-C2
 with sigma of 0.002
 C13-C12 \\sim C14A-C12 \\sim C14-C12 \\sim C13A-C12
 with sigma of 0.002
 O1A-C8A \\sim O1-C8
 with sigma of 0.002
        5. Rigid bond restraints
 C7, N1, C1, C2, C6, C5, C3, C4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N2, C8, C9, C10, C11, O1, N4, C12, C13, C14, N3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C6A, C2A, C1, N1A, C7A, C3, C4, C5
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N1, C5, C1, C2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O1A, N2A, C8A, C9A, C10A, N4A, C12, C11A, C14A, C13A, N3A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Cl1, Cl1A, Pd1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
        6. Uiso/Uaniso restraints and constraints
        Uanis(C6A) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C7A) \\sim Ueq, Uanis(C6)
        \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
        Uanis(Cl1) \\sim Ueq, Uanis(Cl1A) \\sim Ueq: with sigma of 0.01 and sigma for
        terminal atoms of 0.01
        Uanis(O1A) \\sim Ueq, Uanis(C9A) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10A)
        \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C11A) \\sim Ueq, Uanis(C10) \\sim Ueq,
        Uanis(O1) \\sim Ueq, Uanis(C8) \\sim Ueq: with sigma of 0.01 and sigma for
        terminal atoms of 0.01
        Uanis(C8A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.02
        Uanis(N4A) \\sim Ueq, Uanis(N3A) \\sim Ueq, Uanis(N2A) \\sim Ueq, Uanis(N2)
        \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(N4) \\sim Ueq: with sigma of 0.01 and
        sigma for terminal atoms of 0.02
        Uanis(C2) = Uanis(N1A)
        Uanis(C2A) = Uanis(N1)
        7. Others
 Sof(H12A)=Sof(O1A)=Sof(C8A)=Sof(C9A)=Sof(C11A)=Sof(H11A)=Sof(C13A)=Sof(H13D)=
 Sof(H13E)=Sof(H13F)=Sof(C14A)=Sof(H14D)=Sof(H14E)=Sof(H14F)=Sof(C10A)=
 Sof(H10A)=Sof(N4A)=Sof(N3A)=Sof(N2A)=1-FVAR(1)
 Sof(N2)=Sof(N3)=Sof(H12)=Sof(N4)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=
 Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C9)=Sof(C10)=Sof(H10)=Sof(C11)=
 Sof(H11)=Sof(C8)=Sof(O1)=FVAR(1)
 Sof(Cl1A)=1-FVAR(2)
 Sof(Cl1)=FVAR(2)
 Sof(H5B)=Sof(H3B)=Sof(N1A)=Sof(C2A)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=
 Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=1-FVAR(3)
 Sof(C2)=Sof(N1)=Sof(H5A)=Sof(H3A)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=Sof(C7)=
 Sof(H7A)=Sof(H7B)=Sof(H7C)=FVAR(3)
        8.a Ternary CH refined with riding coordinates:
 C12(H12), C12(H12A)
        8.b Aromatic/amide H refined with riding coordinates:
 C5(H5A), C5(H5B), C4(H4), C3(H3A), C3(H3B), C11A(H11A), C10A(H10A), C10(H10),
 C11(H11)
        8.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C13A(H13D,H13E,H13F), C14(H14A,H14B,H14C), C14A(H14D,
 H14E,H14F), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C6A(H6AA,H6AB,H6AC), C7A(H7AA,
 H7AB,H7AC)
;

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 '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'

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 -0.24931(6) -0.57677(2) -0.36062(2) 0.03442(8) Uani 1 1 d . U . . .
Cl2 Cl -0.2623(3) -0.50037(9) -0.24804(4) 0.0519(3) Uani 1 1 d . . . . .
Cl1 Cl -0.3017(7) -0.7822(3) -0.31899(13) 0.0582(13) Uani 0.693(11) 1 d . U P A
1
N2 N -0.2254(7) -0.3939(10) -0.3963(4) 0.0224(16) Uani 0.631(7) 1 d . U P A 1
N3 N -0.2166(10) -0.6157(10) -0.4645(6) 0.0287(14) Uani 0.631(7) 1 d . U P A 1
C2 C -0.1074(6) -0.2306(6) -0.3313(3) 0.0503(12) Uani 0.47(5) 1 d D U P A 1
N1 N -0.3702(6) -0.2348(6) -0.3321(3) 0.0508(13) Uani 0.47(5) 1 d D U P A 1
C1 C -0.2336(8) -0.2840(3) -0.35483(18) 0.0422(7) Uani 1 1 d . U . . .
C5 C -0.3771(8) -0.1339(7) -0.2851(4) 0.0555(14) Uani 1 1 d . U . . .
H5A H -0.470666 -0.101047 -0.268952 0.067 Uiso 0.47(5) 1 calc R U P A 1
H5B H -0.470666 -0.101047 -0.268952 0.067 Uiso 0.53(5) 1 calc R U P A 2
C12 C -0.2284(7) -0.8519(4) -0.4872(2) 0.0512(11) Uani 1 1 d D U . . .
H12 H -0.300766 -0.849772 -0.446906 0.061 Uiso 0.631(7) 1 calc R U P A 1
H12A H -0.151014 -0.852229 -0.449044 0.061 Uiso 0.369(7) 1 calc R U P A 2
C4 C -0.2402(10) -0.0805(4) -0.2613(2) 0.0585(9) Uani 1 1 d . U . . .
H4 H -0.240696 -0.010771 -0.228395 0.07 Uiso 1 1 calc R U . . .
N4 N -0.2004(12) -0.7150(10) -0.5097(5) 0.0379(13) Uani 0.631(7) 1 d . U P A 1
C3 C -0.1143(9) -0.1261(8) -0.2842(4) 0.0620(17) Uani 1 1 d . U . . .
H3A H -0.023495 -0.08733 -0.268492 0.074 Uiso 0.47(5) 1 calc R U P A 1
H3B H -0.023495 -0.08733 -0.268492 0.074 Uiso 0.53(5) 1 calc R U P A 2
O1A O -0.303(2) -0.2745(13) -0.4994(9) 0.065(4) Uani 0.369(7) 1 d D U P A 2
C8A C -0.273(2) -0.3775(14) -0.4682(10) 0.042(3) Uani 0.369(7) 1 d D U P A 2
C9A C -0.2766(15) -0.5087(15) -0.5039(7) 0.031(2) Uani 0.369(7) 1 d . U P A 2
C11A C -0.319(3) -0.678(2) -0.5765(11) 0.067(4) Uani 0.369(7) 1 d . U P A 2
H11A H -0.351425 -0.728719 -0.615506 0.08 Uiso 0.369(7) 1 calc R U P A 2
C13 C -0.0809(10) -0.9099(11) -0.4602(6) 0.067(3) Uani 0.631(7) 1 d D U P A 1
H13A H -0.033939 -0.849043 -0.427091 0.1 Uiso 0.631(7) 1 calc R U P A 1
H13B H -0.013199 -0.925238 -0.499998 0.1 Uiso 0.631(7) 1 calc R U P A 1
H13C H -0.1012 -0.992656 -0.436198 0.1 Uiso 0.631(7) 1 calc R U P A 1
C13A C -0.3842(14) -0.899(2) -0.4645(12) 0.072(5) Uani 0.369(7) 1 d D U P A 2
H13D H -0.455406 -0.885433 -0.503149 0.108 Uiso 0.369(7) 1 calc R U P A 2
H13E H -0.417064 -0.849238 -0.423151 0.108 Uiso 0.369(7) 1 calc R U P A 2
H13F H -0.37977 -0.991677 -0.452682 0.108 Uiso 0.369(7) 1 calc R U P A 2
C14 C -0.2975(16) -0.9353(12) -0.5456(6) 0.072(3) Uani 0.631(7) 1 d D U P A 1
H14A H -0.221974 -0.952096 -0.581969 0.108 Uiso 0.631(7) 1 calc R U P A 1
H14B H -0.382692 -0.888874 -0.566427 0.108 Uiso 0.631(7) 1 calc R U P A 1
H14C H -0.331998 -1.018181 -0.525749 0.108 Uiso 0.631(7) 1 calc R U P A 1
C14A C -0.185(3) -0.927(2) -0.5537(10) 0.080(6) Uani 0.369(7) 1 d D U P A 2
H14D H -0.091927 -0.891493 -0.573012 0.121 Uiso 0.369(7) 1 calc R U P A 2
H14E H -0.265392 -0.91907 -0.588748 0.121 Uiso 0.369(7) 1 calc R U P A 2
H14F H -0.170621 -1.019389 -0.542002 0.121 Uiso 0.369(7) 1 calc R U P A 2
C10A C -0.304(2) -0.5334(19) -0.5707(9) 0.067(4) Uani 0.369(7) 1 d . U P A 2
H10A H -0.31161 -0.471647 -0.607762 0.08 Uiso 0.369(7) 1 calc R U P A 2
C9 C -0.1801(8) -0.5039(8) -0.5029(4) 0.0319(15) Uani 0.631(7) 1 d . U P A 1
C10 C -0.1468(10) -0.5407(9) -0.5730(5) 0.0469(18) Uani 0.631(7) 1 d . U P A 1
H10 H -0.11794 -0.485789 -0.610956 0.056 Uiso 0.631(7) 1 calc R U P A 1
C11 C -0.1650(15) -0.6699(12) -0.5740(6) 0.059(3) Uani 0.631(7) 1 d . U P A 1
H11 H -0.15434 -0.722874 -0.614764 0.071 Uiso 0.631(7) 1 calc R U P A 1
C8 C -0.1919(11) -0.3797(7) -0.4670(4) 0.0324(15) Uani 0.631(7) 1 d D U P A 1
O1 O -0.1812(14) -0.2730(7) -0.4972(4) 0.061(2) Uani 0.631(7) 1 d D U P A 1
N4A N -0.276(3) -0.7168(19) -0.5122(10) 0.052(3) Uani 0.369(7) 1 d . U P A 2
N3A N -0.272(2) -0.609(2) -0.4667(13) 0.041(3) Uani 0.369(7) 1 d . U P A 2
N2A N -0.277(2) -0.3926(18) -0.4027(9) 0.036(3) Uani 0.369(7) 1 d . U P A 2
Cl1A Cl -0.1835(17) -0.7804(7) -0.3193(3) 0.065(3) Uani 0.307(11) 1 d . U P A 2
C6 C 0.033(3) -0.274(4) -0.363(2) 0.069(6) Uani 0.47(5) 1 d D U P A 1
H6A H 0.117669 -0.235293 -0.337457 0.103 Uiso 0.47(5) 1 calc R U P A 1
H6B H 0.036525 -0.247189 -0.412377 0.103 Uiso 0.47(5) 1 calc R U P A 1
H6C H 0.039562 -0.369375 -0.360006 0.103 Uiso 0.47(5) 1 calc R U P A 1
N1A N -0.1074(6) -0.2306(6) -0.3313(3) 0.0503(12) Uani 0.53(5) 1 d D U P A 2
C2A C -0.3702(6) -0.2348(6) -0.3321(3) 0.0508(13) Uani 0.53(5) 1 d D U P A 2
C7 C -0.511(3) -0.311(2) -0.3532(16) 0.054(3) Uani 0.47(5) 1 d D U P A 1
H7A H -0.525419 -0.305017 -0.404271 0.08 Uiso 0.47(5) 1 calc R U P A 1
H7B H -0.598433 -0.274729 -0.329019 0.08 Uiso 0.47(5) 1 calc R U P A 1
H7C H -0.498799 -0.402903 -0.339844 0.08 Uiso 0.47(5) 1 calc R U P A 1
C6A C -0.515(2) -0.279(3) -0.3592(16) 0.065(5) Uani 0.53(5) 1 d D U P A 2
H6AA H -0.527121 -0.371936 -0.349113 0.097 Uiso 0.53(5) 1 calc R U P A 2
H6AB H -0.518498 -0.264738 -0.41021 0.097 Uiso 0.53(5) 1 calc R U P A 2
H6AC H -0.595425 -0.229625 -0.336446 0.097 Uiso 0.53(5) 1 calc R U P A 2
C7A C 0.046(2) -0.289(4) -0.3499(14) 0.064(4) Uani 0.53(5) 1 d D U P A 2
H7AA H 0.119844 -0.262091 -0.314382 0.096 Uiso 0.53(5) 1 calc R U P A 2
H7AB H 0.077657 -0.25668 -0.396269 0.096 Uiso 0.53(5) 1 calc R U P A 2
H7AC H 0.038937 -0.383787 -0.35093 0.096 Uiso 0.53(5) 1 calc R U P A 2



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 Cl2 2.2794(9) . ?
Pd1 Cl1 2.299(3) . ?
Pd1 N2 2.006(10) . ?
Pd1 N3 2.033(12) . ?
Pd1 N3A 2.05(2) . ?
Pd1 N2A 2.067(18) . ?
Pd1 Cl1A 2.307(6) . ?
N2 C1 1.378(11) . ?
N2 C8 1.382(10) . ?
N3 N4 1.340(14) . ?
N3 C9 1.398(14) . ?
C2 C1 1.329(8) . ?
C2 C3 1.398(9) . ?
C2 C6 1.459(18) . ?
N1 C1 1.387(8) . ?
N1 C5 1.369(8) . ?
N1 C7 1.532(18) . ?
C1 N2A 1.489(18) . ?
C1 N1A 1.329(8) . ?
C1 C2A 1.387(8) . ?
C5 H5A 0.95 . ?
C5 H5B 0.95 . ?
C5 C4 1.412(10) . ?
C5 C2A 1.369(8) . ?
C12 H12 1 . ?
C12 H12A 1 . ?
C12 N4 1.490(11) . ?
C12 C13 1.532(6) . ?
C12 C13A 1.531(6) . ?
C12 C14 1.530(6) . ?
C12 C14A 1.531(6) . ?
C12 N4A 1.53(2) . ?
C4 H4 0.95 . ?
C4 C3 1.291(10) . ?
N4 C11 1.343(14) . ?
C3 H3A 0.95 . ?
C3 H3B 0.95 . ?
C3 N1A 1.398(9) . ?
O1A C8A 1.240(6) . ?
C8A C9A 1.51(2) . ?
C8A N2A 1.25(2) . ?
C9A C10A 1.31(2) . ?
C9A N3A 1.25(3) . ?
C11A H11A 0.95 . ?
C11A C10A 1.49(3) . ?
C11A N4A 1.34(3) . ?
C13 H13A 0.98 . ?
C13 H13B 0.98 . ?
C13 H13C 0.98 . ?
C13A H13D 0.98 . ?
C13A H13E 0.98 . ?
C13A H13F 0.98 . ?
C14 H14A 0.98 . ?
C14 H14B 0.98 . ?
C14 H14C 0.98 . ?
C14A H14D 0.98 . ?
C14A H14E 0.98 . ?
C14A H14F 0.98 . ?
C10A H10A 0.95 . ?
C9 C10 1.415(10) . ?
C9 C8 1.450(11) . ?
C10 H10 0.95 . ?
C10 C11 1.336(15) . ?
C11 H11 0.95 . ?
C8 O1 1.240(6) . ?
N4A N3A 1.40(3) . ?
C6 H6A 0.98 . ?
C6 H6B 0.98 . ?
C6 H6C 0.98 . ?
N1A C7A 1.533(18) . ?
C2A C6A 1.458(18) . ?
C7 H7A 0.98 . ?
C7 H7B 0.98 . ?
C7 H7C 0.98 . ?
C6A H6AA 0.98 . ?
C6A H6AB 0.98 . ?
C6A H6AC 0.98 . ?
C7A H7AA 0.98 . ?
C7A H7AB 0.98 . ?
C7A H7AC 0.98 . ?

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
Cl2 Pd1 Cl1 89.01(7) . . ?
Cl2 Pd1 Cl1A 90.33(17) . . ?
N2 Pd1 Cl2 90.0(2) . . ?
N2 Pd1 Cl1 174.4(2) . . ?
N2 Pd1 N3 80.8(4) . . ?
N3 Pd1 Cl2 169.8(3) . . ?
N3 Pd1 Cl1 100.5(3) . . ?
N3A Pd1 Cl2 166.2(5) . . ?
N3A Pd1 N2A 75.9(8) . . ?
N3A Pd1 Cl1A 102.3(6) . . ?
N2A Pd1 Cl2 92.4(5) . . ?
N2A Pd1 Cl1A 171.8(6) . . ?
C1 N2 Pd1 124.5(4) . . ?
C1 N2 C8 118.7(8) . . ?
C8 N2 Pd1 116.7(7) . . ?
N4 N3 Pd1 141.8(9) . . ?
N4 N3 C9 105.3(9) . . ?
C9 N3 Pd1 112.3(7) . . ?
C1 C2 C3 119.6(5) . . ?
C1 C2 C6 117.6(16) . . ?
C3 C2 C6 122.4(16) . . ?
C1 N1 C7 116.8(11) . . ?
C5 N1 C1 121.2(5) . . ?
C5 N1 C7 121.4(12) . . ?
N2 C1 N1 121.5(6) . . ?
C2 C1 N2 119.0(6) . . ?
C2 C1 N1 119.3(3) . . ?
N1A C1 N2A 137.2(9) . . ?
N1A C1 C2A 119.3(3) . . ?
C2A C1 N2A 103.5(9) . . ?
N1 C5 H5A 121.2 . . ?
N1 C5 C4 117.6(6) . . ?
C4 C5 H5A 121.2 . . ?
C4 C5 H5B 121.2 . . ?
C2A C5 H5B 121.2 . . ?
C2A C5 C4 117.6(6) . . ?
N4 C12 H12 107.9 . . ?
N4 C12 C13 108.6(7) . . ?
N4 C12 C14 112.7(7) . . ?
C13 C12 H12 107.9 . . ?
C13A C12 H12A 114.9 . . ?
C14 C12 H12 107.9 . . ?
C14 C12 C13 111.8(8) . . ?
C14A C12 H12A 114.9 . . ?
C14A C12 C13A 107.6(14) . . ?
N4A C12 H12A 114.9 . . ?
N4A C12 C13A 96.8(12) . . ?
N4A C12 C14A 105.8(13) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 C5 120.2(4) . . ?
C3 C4 H4 119.9 . . ?
N3 N4 C12 121.0(9) . . ?
N3 N4 C11 110.3(10) . . ?
C11 N4 C12 128.7(9) . . ?
C2 C3 H3A 118.9 . . ?
C4 C3 C2 122.1(7) . . ?
C4 C3 H3A 118.9 . . ?
C4 C3 H3B 118.9 . . ?
C4 C3 N1A 122.1(7) . . ?
N1A C3 H3B 118.9 . . ?
O1A C8A C9A 122.8(16) . . ?
O1A C8A N2A 124.9(19) . . ?
N2A C8A C9A 109.6(14) . . ?
C10A C9A C8A 127.5(14) . . ?
N3A C9A C8A 118.7(14) . . ?
N3A C9A C10A 113.1(18) . . ?
C10A C11A H11A 129.2 . . ?
N4A C11A H11A 129.2 . . ?
N4A C11A C10A 101.6(18) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C13A H13D 109.5 . . ?
C12 C13A H13E 109.5 . . ?
C12 C13A H13F 109.5 . . ?
H13D C13A H13E 109.5 . . ?
H13D C13A H13F 109.5 . . ?
H13E C13A H13F 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C14A H14D 109.5 . . ?
C12 C14A H14E 109.5 . . ?
C12 C14A H14F 109.5 . . ?
H14D C14A H14E 109.5 . . ?
H14D C14A H14F 109.5 . . ?
H14E C14A H14F 109.5 . . ?
C9A C10A C11A 106.3(18) . . ?
C9A C10A H10A 126.9 . . ?
C11A C10A H10A 126.9 . . ?
N3 C9 C10 108.7(8) . . ?
N3 C9 C8 117.3(7) . . ?
C10 C9 C8 133.9(8) . . ?
C9 C10 H10 127.7 . . ?
C11 C10 C9 104.7(9) . . ?
C11 C10 H10 127.7 . . ?
N4 C11 H11 124.5 . . ?
C10 C11 N4 110.9(10) . . ?
C10 C11 H11 124.5 . . ?
N2 C8 C9 112.3(7) . . ?
O1 C8 N2 124.0(9) . . ?
O1 C8 C9 123.6(7) . . ?
C11A N4A C12 129.4(17) . . ?
C11A N4A N3A 109.5(18) . . ?
N3A N4A C12 121.0(17) . . ?
C9A N3A Pd1 115.2(15) . . ?
C9A N3A N4A 107.4(19) . . ?
N4A N3A Pd1 137.3(16) . . ?
C1 N2A Pd1 114.6(9) . . ?
C8A N2A Pd1 119.5(14) . . ?
C8A N2A C1 120.3(15) . . ?
C2 C6 H6A 109.5 . . ?
C2 C6 H6B 109.5 . . ?
C2 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C1 N1A C3 119.6(5) . . ?
C1 N1A C7A 121.3(13) . . ?
C3 N1A C7A 119.0(13) . . ?
C1 C2A C6A 123.5(12) . . ?
C5 C2A C1 121.2(5) . . ?
C5 C2A C6A 115.1(12) . . ?
N1 C7 H7A 109.5 . . ?
N1 C7 H7B 109.5 . . ?
N1 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C2A C6A H6AA 109.5 . . ?
C2A C6A H6AB 109.5 . . ?
C2A C6A H6AC 109.5 . . ?
H6AA C6A H6AB 109.5 . . ?
H6AA C6A H6AC 109.5 . . ?
H6AB C6A H6AC 109.5 . . ?
N1A C7A H7AA 109.5 . . ?
N1A C7A H7AB 109.5 . . ?
N1A C7A H7AC 109.5 . . ?
H7AA C7A H7AB 109.5 . . ?
H7AA C7A H7AC 109.5 . . ?
H7AB C7A H7AC 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
Pd1 N2 C1 C2 97.0(6) . . . . ?
Pd1 N2 C1 N1 -77.3(7) . . . . ?
Pd1 N2 C8 C9 0.0(9) . . . . ?
Pd1 N2 C8 O1 176.3(9) . . . . ?
Pd1 N3 N4 C12 9.7(17) . . . . ?
Pd1 N3 N4 C11 -173.3(10) . . . . ?
Pd1 N3 C9 C10 175.1(6) . . . . ?
Pd1 N3 C9 C8 -8.5(9) . . . . ?
N3 N4 C11 C10 4.0(16) . . . . ?
N3 C9 C10 C11 0.3(12) . . . . ?
N3 C9 C8 N2 5.7(11) . . . . ?
N3 C9 C8 O1 -170.6(10) . . . . ?
N1 C5 C4 C3 0.4(7) . . . . ?
C1 N2 C8 C9 177.2(7) . . . . ?
C1 N2 C8 O1 -6.5(14) . . . . ?
C1 C2 C3 C4 1.3(11) . . . . ?
C1 N1 C5 C4 0.9(9) . . . . ?
C5 N1 C1 N2 173.1(6) . . . . ?
C5 N1 C1 C2 -1.2(7) . . . . ?
C5 C4 C3 C2 -1.6(9) . . . . ?
C5 C4 C3 N1A -1.6(9) . . . . ?
C12 N4 C11 C10 -179.2(10) . . . . ?
C12 N4A N3A Pd1 -13(3) . . . . ?
C12 N4A N3A C9A 162.2(17) . . . . ?
C4 C5 C2A C1 0.9(9) . . . . ?
C4 C5 C2A C6A -175.1(15) . . . . ?
C4 C3 N1A C1 1.3(11) . . . . ?
C4 C3 N1A C7A -173.5(17) . . . . ?
N4 N3 C9 C10 2.0(10) . . . . ?
N4 N3 C9 C8 178.4(8) . . . . ?
C3 C2 C1 N2 -174.4(6) . . . . ?
C3 C2 C1 N1 0.1(7) . . . . ?
O1A C8A C9A C10A 3(3) . . . . ?
O1A C8A C9A N3A -167(2) . . . . ?
O1A C8A N2A Pd1 172.4(18) . . . . ?
O1A C8A N2A C1 -35(3) . . . . ?
C8A C9A C10A C11A -170.8(19) . . . . ?
C8A C9A N3A Pd1 -3(2) . . . . ?
C8A C9A N3A N4A -179.7(17) . . . . ?
C9A C8A N2A Pd1 11(2) . . . . ?
C9A C8A N2A C1 163.4(13) . . . . ?
C11A N4A N3A Pd1 169.8(18) . . . . ?
C11A N4A N3A C9A -15(3) . . . . ?
C13 C12 N4 N3 -90.7(10) . . . . ?
C13 C12 N4 C11 92.8(13) . . . . ?
C13A C12 N4A C11A -91(3) . . . . ?
C13A C12 N4A N3A 92(2) . . . . ?
C14 C12 N4 N3 144.9(10) . . . . ?
C14 C12 N4 C11 -31.5(15) . . . . ?
C14A C12 N4A C11A 19(3) . . . . ?
C14A C12 N4A N3A -157(2) . . . . ?
C10A C9A N3A Pd1 -174.8(14) . . . . ?
C10A C9A N3A N4A 9(2) . . . . ?
C10A C11A N4A C12 -163(2) . . . . ?
C10A C11A N4A N3A 14(3) . . . . ?
C9 N3 N4 C12 179.4(8) . . . . ?
C9 N3 N4 C11 -3.6(12) . . . . ?
C9 C10 C11 N4 -2.6(15) . . . . ?
C10 C9 C8 N2 -179.0(8) . . . . ?
C10 C9 C8 O1 4.7(16) . . . . ?
C8 N2 C1 C2 -80.0(8) . . . . ?
C8 N2 C1 N1 105.7(8) . . . . ?
C8 C9 C10 C11 -175.2(11) . . . . ?
N4A C11A C10A C9A -9(3) . . . . ?
N3A C9A C10A C11A 0(2) . . . . ?
N2A C1 N1A C3 -179.3(11) . . . . ?
N2A C1 N1A C7A -5(2) . . . . ?
N2A C1 C2A C5 178.4(8) . . . . ?
N2A C1 C2A C6A -5.9(18) . . . . ?
N2A C8A C9A C10A 165.3(19) . . . . ?
N2A C8A C9A N3A -5(2) . . . . ?
C6 C2 C1 N2 13(2) . . . . ?
C6 C2 C1 N1 -173(2) . . . . ?
C6 C2 C3 C4 174(2) . . . . ?
N1A C1 N2A Pd1 75.1(14) . . . . ?
N1A C1 N2A C8A -79(2) . . . . ?
N1A C1 C2A C5 -1.2(7) . . . . ?
N1A C1 C2A C6A 174.6(17) . . . . ?
C2A C1 N2A Pd1 -104.4(9) . . . . ?
C2A C1 N2A C8A 101.8(18) . . . . ?
C2A C1 N1A C3 0.1(7) . . . . ?
C2A C1 N1A C7A 174.8(16) . . . . ?
C2A C5 C4 C3 0.4(7) . . . . ?
C7 N1 C1 N2 2.1(14) . . . . ?
C7 N1 C1 C2 -172.2(13) . . . . ?
C7 N1 C5 C4 171.6(13) . . . . ?


#----------------------------------------------------------------------------#
#                   VALIDATION REPLY FORM                                    #
#----------------------------------------------------------------------------#

_vrf_STRVA01_23MA063_MA-055      
;
PROBLEM: Flack test results are ambiguous.
RESPONSE: No solution was found using a centro-symmetric space group.
The structure was refined as an inversion twin.
;

#----------------------------------------------------------------------------#
#                   SHELX RES FILE                                           #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   SHELX HKL FILE                                           #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   SHELX FAB FILE                                           #
#----------------------------------------------------------------------------#

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
####################################################################### 
# 
# 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_23MA069_MA-013
_database_code_depnum_ccdc_archive 'CCDC 2394913'
loop_
_audit_author_name
_audit_author_address
'Lorraine Malaspina'
;University of Bern
Switzerland
;
_audit_update_record             
;
2024-10-30 deposited with the CCDC.	2024-12-18 downloaded from the CCDC.
;

_audit_creation_date             2023-10-16T15:51:08-00:00

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         'C12 H14 Cl2 N4 O Pd'
_chemical_formula_sum            'C12 H14 Cl2 N4 O Pd'
_chemical_formula_weight         407.57

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P c c n'
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_Int_Tables_number      56
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z-1/2'
'-x-1/2, y, z-1/2'

_cell_length_a                   10.97050(13)
_cell_length_b                   23.0363(2)
_cell_length_c                   14.07250(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3556.40(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    173.00(10)
_cell_measurement_reflns_used    71695
_cell_measurement_theta_min      2.503
_cell_measurement_theta_max      33.546

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.314
_exptl_crystal_size_mid          0.224
_exptl_crystal_size_min          0.184
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_F_000             1616
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -1 0 0.1448
0 1 0 0.0541
-1 -1 1 0.1297
0 -1 -1 0.1101
0 1 1 0.1408
-1 -1 0 0.0615
1 1 0 0.1266
-1 0 1 0.1208
1 0 -1 0.1018
-1 -1 -1 0.0868
1 1 1 0.109
1 0 0 0.1196
-1 0 -1 0.0877
-1 1 1 0.1235
1 0 1 0.1039
1 -1 -1 0.1039
-1 1 0 0.0671
1 -1 1 0.1234
-1 1 -1 0.0984
0 0 -1 0.1326
0 0 1 0.1708
0 -1 1 0.1619
2 -24 13 0.1376
4 -20 -15 0.1063
-8 -24 -9 0.0749
-12 -21 0 0.0684

loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0 -0.9987 0.0001 0.0282 -0.0073 0.0099
0 0.9987 -0.0001 -0.0282 0.0073 -0.0099
-0.9988 -0.9993 0.9989 0.0607 0.0306 -0.055
-0.0002 -0.9985 -0.9987 0.0174 0.0124 0.055
0.0002 0.9985 0.9987 -0.0174 -0.0124 -0.055
-0.9989 -0.9991 0.0001 0.05 0.0502 -0.0099
0.9989 0.9991 -0.0001 -0.05 -0.0502 0.0099
-0.9987 -0.0005 0.9988 0.0325 0.0378 -0.0649
0.9987 0.0005 -0.9988 -0.0325 -0.0378 0.0649
-0.9991 -0.9989 -0.9988 0.0392 0.0699 0.0352
0.9991 0.9989 0.9988 -0.0392 -0.0699 -0.0352
0.9989 0.0004 0 -0.0218 -0.0575 0.0198
-0.9991 -0.0002 -0.9989 0.011 0.0771 0.0253
-0.9987 0.9982 0.9987 0.0043 0.0451 -0.0748
0.9991 0.0002 0.9989 -0.011 -0.0771 -0.0253
0.9987 -0.9982 -0.9987 -0.0043 -0.0451 0.0748
-0.9989 0.9984 -0.0001 -0.0064 0.0647 -0.0297
0.999 -0.9985 0.999 0.0172 -0.0844 -0.0154
-0.999 0.9985 -0.999 -0.0172 0.0844 0.0154
-0.0002 0.0002 -0.9988 -0.0107 0.0196 0.0451
0.0002 -0.0002 0.9988 0.0107 -0.0196 -0.0451
0.0001 -0.9989 0.999 0.0389 -0.0269 -0.0352
1.9989 -23.971 12.9876 0.7729 -0.5448 -0.309
3.9924 -19.9702 -14.9805 0.3156 -0.0805 0.9536
-7.9936 -23.9705 -8.9872 0.7542 0.4622 0.4848
-11.9877 -20.9775 0.002 0.8535 0.537 -0.0301


#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.344
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
        CrysAlisPro 1.171.42.89a (Rigaku Oxford Diffraction, 2023)
        Numerical absorption correction based on gaussian integration over
        a multifaceted crystal model
        Empirical absorption correction using spherical harmonics,
        implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.704
_exptl_absorpt_correction_T_max  1
_shelx_estimated_absorpt_T_min   0.678
_shelx_estimated_absorpt_T_max   0.79
_oxdiff_exptl_absorpt_empirical_details 
;
        Empirical correction (ABSPACK) includes:
        - Absorption correction using spherical harmonics
        - Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.25
_oxdiff_exptl_absorpt_empirical_full_min 0.815

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_diffrn_ambient_temperature      173.00(10)
_diffrn_ambient_environment      N~2~
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_detector_area_resol_mean 10
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_ub_11      -0.0217934
_diffrn_orient_matrix_ub_12      -0.0282309
_diffrn_orient_matrix_ub_13      0.0107587
_diffrn_orient_matrix_ub_21      -0.0575342
_diffrn_orient_matrix_ub_22      0.0072757
_diffrn_orient_matrix_ub_23      -0.0196613
_diffrn_orient_matrix_ub_31      0.0198503
_diffrn_orient_matrix_ub_32      -0.0099151
_diffrn_orient_matrix_ub_33      -0.0451484
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix-Arc 100'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_number            102018
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.056
_diffrn_reflns_theta_max         30.506
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1
_reflns_Friedel_coverage         0
_reflns_number_total             5437
_reflns_number_gt                5064
_reflns_threshold_expression     'I > 2σ(I)'
_diffrn_measurement_details      
;
        List of Runs (angles in degrees, time in seconds):
  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
        --------------------------------------------------------------------------
  1  ω    -18.00  55.00   0.50    0.60    --   13.29 -99.00 112.00  146
  2  ω    -28.00  21.00   0.50    0.60    --   13.29  99.00-141.00   98
  3  ω    -55.00  21.00   0.50    0.60    --  -13.44  99.00-141.00  152
  4  ω    -19.00  29.00   0.50    0.60    --  -13.44 -99.00 112.00   96
  5  ω    -25.00  94.00   0.50    0.60    --   13.29  19.00  90.00  238
  6  ω    -87.00 -42.00   0.50    0.60    --  -13.44-178.00  60.00   90
  7  ω    -94.00   7.00   0.50    0.60    --  -13.44 -38.00-120.00  202
  8  ω    -19.00  29.00   0.50    0.60    --  -13.44 -99.00-120.00   96
  9  ω    -90.00   8.00   0.50    0.60    --  -13.44 -57.00   0.00  196
 10  ω     -8.00  90.00   0.50    0.60    --   13.29  57.00-180.00  196
 11  ω    -18.00  37.00   0.50    0.60    --   13.29 -99.00  30.00  110
 12  ω    -87.00 -42.00   0.50    0.60    --  -13.44-178.00-120.00   90
;

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'

#----------------------------------------------------------------------------#
#                   TWINNING                                                 #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   SQUEEZE                                                  #
#----------------------------------------------------------------------------#

loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.118 0.038 0.22 58.6 17.3 0
2 0.118 -0.038 0.78 58.6 16.4 0
3 -0.118 0.462 0.72 58.6 16.4 0
4 0.118 0.538 0.28 58.6 17.4 0
5 0.25 0.25 0.49 66.6 17 0
6 0.25 0.25 -0.01 66.6 17.9 0
7 0.382 0.538 0.78 58.6 17.1 0
8 0.382 0.962 0.28 58.6 16.6 0
9 0.618 0.038 0.72 58.6 17.2 0
10 0.618 0.462 0.22 58.6 16.7 0
11 0.75 0.75 0.51 66.6 17.8 0
12 0.75 0.75 0.01 66.6 17 0

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     dual
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_shelx_SHELXL_version_number     2018/3
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0265P)²+2.4681P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         5437
_refine_ls_number_parameters     184
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0247
_refine_ls_R_factor_gt           0.0227
_refine_ls_wR_factor_ref         0.0611
_refine_ls_wR_factor_gt          0.0603
_refine_ls_goodness_of_fit_ref   1.11
_refine_ls_restrained_S_all      1.11
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.52
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.061

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#

_olex2_refinement_description    
;
        1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
        2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C8(H8), C10(H10), C3(H3), C9(H9)
        2.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C11(H11A,H11B,H11C), C1(H1A,H1B,H1C)
;

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 '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'

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 0.45048(2) 0.62553(2) 0.39040(2) 0.02344(4) Uani 1 1 d . . . . .
Cl1 Cl 0.27561(4) 0.66507(2) 0.33025(3) 0.03504(9) Uani 1 1 d . . . . .
Cl2 Cl 0.34145(4) 0.59242(2) 0.51896(3) 0.03340(9) Uani 1 1 d . . . . .
O1 O 0.73614(12) 0.64651(7) 0.20518(11) 0.0443(3) Uani 1 1 d . . . . .
N3 N 0.54840(12) 0.65338(6) 0.27723(11) 0.0298(3) Uani 1 1 d . . . . .
N2 N 0.61870(12) 0.59409(6) 0.42362(10) 0.0280(3) Uani 1 1 d . . . . .
N1 N 0.67332(14) 0.56256(6) 0.49232(11) 0.0323(3) Uani 1 1 d . . . . .
C7 C 0.45662(14) 0.65817(8) 0.12299(11) 0.0266(3) Uani 1 1 d . . . . .
N4 N 0.49283(15) 0.74506(7) 0.21011(11) 0.0364(3) Uani 1 1 d . . . . .
C6 C 0.50014(14) 0.68561(7) 0.20247(11) 0.0266(3) Uani 1 1 d . . . . .
C4 C 0.70308(15) 0.60231(7) 0.35582(13) 0.0308(3) Uani 1 1 d . . . . .
C2 C 0.78955(17) 0.55083(8) 0.46776(15) 0.0397(4) Uani 1 1 d . . . . .
H2 H 0.84607 0.529044 0.504423 0.048 Uiso 1 1 calc R U . . .
C5 C 0.66573(15) 0.63616(7) 0.27129(13) 0.0313(3) Uani 1 1 d . . . . .
C8 C 0.40747(17) 0.69008(9) 0.04994(13) 0.0368(4) Uani 1 1 d . . . . .
H8 H 0.378038 0.671124 -0.005454 0.044 Uiso 1 1 calc R U . . .
C10 C 0.44260(18) 0.77664(9) 0.13734(16) 0.0402(4) Uani 1 1 d . . . . .
H10 H 0.436713 0.817651 0.142684 0.048 Uiso 1 1 calc R U . . .
C3 C 0.81252(17) 0.57563(9) 0.38087(15) 0.0385(4) Uani 1 1 d . . . . .
H3 H 0.886417 0.574807 0.345702 0.046 Uiso 1 1 calc R U . . .
C12 C 0.45942(19) 0.59365(9) 0.11819(15) 0.0409(4) Uani 1 1 d . . . . .
H12A H 0.54281 0.579969 0.12924 0.061 Uiso 1 1 calc R U . . .
H12B H 0.432041 0.580932 0.055258 0.061 Uiso 1 1 calc R U . . .
H12C H 0.405263 0.577569 0.166911 0.061 Uiso 1 1 calc R U . . .
C9 C 0.40098(18) 0.74963(9) 0.05727(14) 0.0419(4) Uani 1 1 d . . . . .
H9 H 0.367626 0.771868 0.006716 0.05 Uiso 1 1 calc R U . . .
C11 C 0.5369(2) 0.77471(9) 0.29772(15) 0.0439(4) Uani 1 1 d . . . . .
H11A H 0.488614 0.761695 0.352316 0.066 Uiso 1 1 calc R U . . .
H11B H 0.528083 0.816803 0.290285 0.066 Uiso 1 1 calc R U . . .
H11C H 0.622864 0.765139 0.308186 0.066 Uiso 1 1 calc R U . . .
C1 C 0.61475(19) 0.54787(9) 0.58157(13) 0.0386(4) Uani 1 1 d . . . . .
H1A H 0.59724 0.583482 0.617121 0.058 Uiso 1 1 calc R U . . .
H1B H 0.669019 0.523016 0.619061 0.058 Uiso 1 1 calc R U . . .
H1C H 0.538444 0.527168 0.568817 0.058 Uiso 1 1 calc R U . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 Cl1 2.2861(4) . ?
Pd1 Cl2 2.2991(4) . ?
Pd1 N3 2.0253(14) . ?
Pd1 N2 2.0369(13) . ?
O1 C5 1.232(2) . ?
N3 C6 1.392(2) . ?
N3 C5 1.350(2) . ?
N2 N1 1.3496(19) . ?
N2 C4 1.343(2) . ?
N1 C2 1.349(2) . ?
N1 C1 1.451(3) . ?
C7 C6 1.370(2) . ?
C7 C8 1.374(2) . ?
C7 C12 1.488(3) . ?
N4 C6 1.376(2) . ?
N4 C10 1.372(2) . ?
N4 C11 1.490(3) . ?
C4 C5 1.480(2) . ?
C4 C3 1.394(2) . ?
C2 H2 0.95 . ?
C2 C3 1.373(3) . ?
C8 H8 0.95 . ?
C8 C9 1.378(3) . ?
C10 H10 0.95 . ?
C10 C9 1.366(3) . ?
C3 H3 0.95 . ?
C12 H12A 0.98 . ?
C12 H12B 0.98 . ?
C12 H12C 0.98 . ?
C9 H9 0.95 . ?
C11 H11A 0.98 . ?
C11 H11B 0.98 . ?
C11 H11C 0.98 . ?
C1 H1A 0.98 . ?
C1 H1B 0.98 . ?
C1 H1C 0.98 . ?

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
Cl1 Pd1 Cl2 89.253(16) . . ?
N3 Pd1 Cl1 91.59(4) . . ?
N3 Pd1 Cl2 178.96(4) . . ?
N3 Pd1 N2 79.19(6) . . ?
N2 Pd1 Cl1 170.73(4) . . ?
N2 Pd1 Cl2 99.95(4) . . ?
C6 N3 Pd1 124.16(10) . . ?
C5 N3 Pd1 117.49(12) . . ?
C5 N3 C6 118.20(15) . . ?
N1 N2 Pd1 139.29(12) . . ?
C4 N2 Pd1 114.30(11) . . ?
C4 N2 N1 106.19(14) . . ?
N2 N1 C1 123.31(15) . . ?
C2 N1 N2 110.12(16) . . ?
C2 N1 C1 126.43(15) . . ?
C6 C7 C8 120.05(17) . . ?
C6 C7 C12 119.37(15) . . ?
C8 C7 C12 120.56(16) . . ?
C6 N4 C11 120.13(16) . . ?
C10 N4 C6 119.53(17) . . ?
C10 N4 C11 120.33(17) . . ?
C7 C6 N3 120.21(15) . . ?
C7 C6 N4 120.16(15) . . ?
N4 C6 N3 119.59(15) . . ?
N2 C4 C5 117.03(14) . . ?
N2 C4 C3 110.61(16) . . ?
C3 C4 C5 132.36(17) . . ?
N1 C2 H2 125.7 . . ?
N1 C2 C3 108.56(16) . . ?
C3 C2 H2 125.7 . . ?
O1 C5 N3 125.99(17) . . ?
O1 C5 C4 122.35(16) . . ?
N3 C5 C4 111.66(15) . . ?
C7 C8 H8 120.1 . . ?
C7 C8 C9 119.80(18) . . ?
C9 C8 H8 120.1 . . ?
N4 C10 H10 119.7 . . ?
C9 C10 N4 120.58(18) . . ?
C9 C10 H10 119.7 . . ?
C4 C3 H3 127.7 . . ?
C2 C3 C4 104.51(17) . . ?
C2 C3 H3 127.7 . . ?
C7 C12 H12A 109.5 . . ?
C7 C12 H12B 109.5 . . ?
C7 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C8 C9 H9 120.1 . . ?
C10 C9 C8 119.88(18) . . ?
C10 C9 H9 120.1 . . ?
N4 C11 H11A 109.5 . . ?
N4 C11 H11B 109.5 . . ?
N4 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 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
Pd1 N3 C6 C7 -92.27(17) . . . . ?
Pd1 N3 C6 N4 85.66(18) . . . . ?
Pd1 N3 C5 O1 176.02(16) . . . . ?
Pd1 N3 C5 C4 -4.15(19) . . . . ?
Pd1 N2 N1 C2 173.42(14) . . . . ?
Pd1 N2 N1 C1 -10.5(3) . . . . ?
Pd1 N2 C4 C5 4.37(19) . . . . ?
Pd1 N2 C4 C3 -175.32(12) . . . . ?
N2 N1 C2 C3 0.5(2) . . . . ?
N2 C4 C5 O1 179.60(17) . . . . ?
N2 C4 C5 N3 -0.2(2) . . . . ?
N2 C4 C3 C2 0.0(2) . . . . ?
N1 N2 C4 C5 180.00(14) . . . . ?
N1 N2 C4 C3 0.30(19) . . . . ?
N1 C2 C3 C4 -0.3(2) . . . . ?
C7 C8 C9 C10 -0.5(3) . . . . ?
N4 C10 C9 C8 1.1(3) . . . . ?
C6 N3 C5 O1 0.3(3) . . . . ?
C6 N3 C5 C4 -179.82(14) . . . . ?
C6 C7 C8 C9 -0.6(3) . . . . ?
C6 N4 C10 C9 -0.6(3) . . . . ?
C4 N2 N1 C2 -0.47(19) . . . . ?
C4 N2 N1 C1 175.58(16) . . . . ?
C5 N3 C6 C7 83.1(2) . . . . ?
C5 N3 C6 N4 -98.97(19) . . . . ?
C5 C4 C3 C2 -179.67(18) . . . . ?
C8 C7 C6 N3 179.06(15) . . . . ?
C8 C7 C6 N4 1.1(2) . . . . ?
C10 N4 C6 N3 -178.45(15) . . . . ?
C10 N4 C6 C7 -0.5(2) . . . . ?
C3 C4 C5 O1 -0.8(3) . . . . ?
C3 C4 C5 N3 179.38(19) . . . . ?
C12 C7 C6 N3 1.1(2) . . . . ?
C12 C7 C6 N4 -176.83(16) . . . . ?
C12 C7 C8 C9 177.30(18) . . . . ?
C11 N4 C6 N3 0.3(2) . . . . ?
C11 N4 C6 C7 178.22(16) . . . . ?
C11 N4 C10 C9 -179.35(18) . . . . ?
C1 N1 C2 C3 -175.44(17) . . . . ?


#----------------------------------------------------------------------------#
#                   VALIDATION REPLY FORM                                    #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   SHELX RES FILE                                           #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   SHELX HKL AND FAB FILE                                   #
#----------------------------------------------------------------------------#


# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
