# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_hm_233b_2
_database_code_depnum_ccdc_archive 'CCDC 2094617'
loop_
_audit_author_name
_audit_author_address
'Hanna K. Maliszewska'
;University of East Anglia
United Kingdom
;
_audit_update_record             
;
2021-07-06 deposited with the CCDC.	2021-10-28 downloaded from the CCDC.
;
_audit_creation_date             2021-02-02
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C25 H26 Cl2 N2 Pd'
_chemical_formula_sum            'C25 H26 Cl2 N2 Pd'
_chemical_formula_weight         531.78
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C100 H104 Cl8 N8 Pd4 '
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'
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           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   9.3560(3)
_cell_length_b                   14.1423(4)
_cell_length_c                   17.5530(5)
_cell_angle_alpha                90
_cell_angle_beta                 103.017(3)
_cell_angle_gamma                90
_cell_volume                     2262.85(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    21971
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      31.1750
_cell_measurement_theta_min      2.2200
_shelx_estimated_absorpt_T_max   0.980
_shelx_estimated_absorpt_T_min   0.718
_exptl_absorpt_coefficient_mu    1.071
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55327
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1080
_exptl_crystal_recrystallization_method 
'vapour diffusion of dichloromethane/MeOH solution and n-Hex at 4 °C'
_exptl_crystal_size_max          0.332
_exptl_crystal_size_mid          0.286
_exptl_crystal_size_min          0.019
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.799
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            26885
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.799
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.997
_diffrn_reflns_theta_min         2.234
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.799
_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  11.00   0.50   11.71    --   -4.50 -58.00 -44.00  176
  2  ω      0.00  26.00   0.50   11.71    --   -4.50 -99.00   0.00   52
  3  ω    -21.00   5.00   0.50   11.71    --   -4.50 -77.00  60.00   52
  4  ω      2.00  28.00   0.50   11.71    --   -4.50 -99.00 120.00   52
  5  ω    -20.00  68.00   0.50   11.71    --   -4.50  58.00  97.00  176
  6  ω    -10.00  47.00   0.50   11.71    --    4.11  57.00 120.00  114
  7  ω      2.00  28.00   0.50   11.71    --    4.11 -99.00-150.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0258246000
_diffrn_orient_matrix_UB_12      -0.0309322000
_diffrn_orient_matrix_UB_13      -0.0257671000
_diffrn_orient_matrix_UB_21      -0.0728686000
_diffrn_orient_matrix_UB_22      -0.0154838000
_diffrn_orient_matrix_UB_23      -0.0156604000
_diffrn_orient_matrix_UB_31      -0.0089089000
_diffrn_orient_matrix_UB_32      0.0363229000
_diffrn_orient_matrix_UB_33      -0.0284765000
_diffrn_oxdiff_digest_frames     
;
019446f0bfe512f9b8df72e988ff815421000258f1f
;
_diffrn_oxdiff_digest_hkl        
;
019fc68e755b3772f4203a70db6594ba45e637
;
_diffrn_radiation_collimation    0.3
_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_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5379
_reflns_number_total             5767
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.646
_refine_diff_density_min         -0.715
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         5767
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0262
_refine_ls_R_factor_gt           0.0240
_refine_ls_restrained_S_all      1.063
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0210P)²+2.4440P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0567
_refine_ls_wR_factor_ref         0.0574
_refine_special_details          ?
_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:
 C00B(H00B), C00D(H00D), C00G(H00G), C00H(H00H), C00I(H00I), C00J(H00J),
 C00K(H00K), C00N(H00N), C00P(H00P), C00R(H00S), C00T(H00W)
2.b Idealised Me refined as rotating group:
 C00M(H00A,H00C,H00E), C00O(H00F,H00L,H00M), C00Q(H00O,H00Q,H00R), C00S(H00T,
 H00U,H00V), C00U(H00X,H00Y,H)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd01 Pd 0.23589(2) 0.26030(2) 0.45262(2) 0.01033(4) Uani 1 1 d . . . . .
Cl02 Cl -0.00098(5) 0.27419(3) 0.47280(2) 0.01491(8) Uani 1 1 d . . . . .
Cl03 Cl 0.45436(5) 0.23306(3) 0.41466(3) 0.01711(9) Uani 1 1 d . . . . .
N004 N 0.25032(16) 0.12873(10) 0.49954(8) 0.0124(3) Uani 1 1 d . . . . .
N005 N 0.26346(16) 0.40353(10) 0.44580(8) 0.0121(3) Uani 1 1 d . . . . .
C006 C 0.29686(18) 0.44507(12) 0.51805(10) 0.0121(3) Uani 1 1 d . . . . .
C007 C 0.34975(18) 0.29868(12) 0.59236(9) 0.0122(3) Uani 1 1 d . . . . .
C008 C 0.34136(19) 0.12590(12) 0.57181(10) 0.0124(3) Uani 1 1 d . . . . .
C009 C 0.41219(19) 0.21482(12) 0.60723(9) 0.0124(3) Uani 1 1 d . . . . .
C00A C 0.29301(18) 0.38463(11) 0.58769(9) 0.0114(3) Uani 1 1 d . . . . .
C00B C 0.3024(2) 0.55015(13) 0.38646(11) 0.0172(3) Uani 1 1 d . . . . .
H00B H 0.303231 0.584860 0.341552 0.021 Uiso 1 1 calc R . . . .
C00C C 0.56143(19) 0.20906(12) 0.66104(10) 0.0127(3) Uani 1 1 d . . . . .
C00D C 0.8228(2) 0.18341(13) 0.68071(11) 0.0178(4) Uani 1 1 d . . . . .
H00D H 0.903756 0.167253 0.660924 0.021 Uiso 1 1 calc R . . . .
C00E C 0.1779(2) 0.05039(12) 0.46739(10) 0.0153(3) Uani 1 1 d . . . . .
C00F C 0.21711(19) 0.41975(12) 0.65224(10) 0.0129(3) Uani 1 1 d . . . . .
C00G C 0.6826(2) 0.18166(12) 0.63216(10) 0.0156(3) Uani 1 1 d . . . . .
H00G H 0.669787 0.162229 0.580445 0.019 Uiso 1 1 calc R . . . .
C00H C 0.33391(19) 0.54040(12) 0.52510(10) 0.0146(3) Uani 1 1 d . . . . .
H00H H 0.357138 0.568657 0.574183 0.018 Uiso 1 1 calc R . . . .
C00I C 0.3362(2) 0.59336(13) 0.45879(11) 0.0182(4) Uani 1 1 d . . . . .
H00I H 0.360224 0.657246 0.463073 0.022 Uiso 1 1 calc R . . . .
C00J C 0.7212(2) 0.23351(13) 0.78827(11) 0.0182(4) Uani 1 1 d . . . . .
H00J H 0.733762 0.248980 0.840859 0.022 Uiso 1 1 calc R . . . .
C00K C 0.5813(2) 0.23482(12) 0.73970(10) 0.0154(3) Uani 1 1 d . . . . .
H00K H 0.501156 0.252794 0.759490 0.019 Uiso 1 1 calc R . . . .
C00L C 0.26712(19) 0.45422(12) 0.38100(10) 0.0140(3) Uani 1 1 d . . . . .
C00M C 0.3314(2) 0.46955(13) 0.71699(10) 0.0169(3) Uani 1 1 d . . . . .
H00A H 0.408398 0.425916 0.738806 0.025 Uiso 1 1 calc GR . . . .
H00C H 0.284938 0.491060 0.757314 0.025 Uiso 1 1 calc GR . . . .
H00E H 0.372083 0.522642 0.695107 0.025 Uiso 1 1 calc GR . . . .
C00N C 0.8415(2) 0.20936(13) 0.75887(12) 0.0199(4) Uani 1 1 d . . . . .
H00N H 0.934993 0.210447 0.791309 0.024 Uiso 1 1 calc R . . . .
C00O C 0.1545(2) 0.33385(13) 0.68770(11) 0.0184(4) Uani 1 1 d . . . . .
H00F H 0.088463 0.299954 0.647064 0.028 Uiso 1 1 calc GR . . . .
H00L H 0.102608 0.355119 0.725879 0.028 Uiso 1 1 calc GR . . . .
H00M H 0.233312 0.292931 0.712266 0.028 Uiso 1 1 calc GR . . . .
C00P C 0.3669(2) 0.04096(12) 0.61261(11) 0.0163(3) Uani 1 1 d . . . . .
H00P H 0.432758 0.038300 0.660917 0.020 Uiso 1 1 calc R . . . .
C00Q C 0.0891(2) 0.48662(13) 0.61861(11) 0.0183(4) Uani 1 1 d . . . . .
H00O H 0.125976 0.542347 0.598372 0.027 Uiso 1 1 calc GR . . . .
H00Q H 0.040328 0.504104 0.659144 0.027 Uiso 1 1 calc GR . . . .
H00R H 0.020910 0.455220 0.577292 0.027 Uiso 1 1 calc GR . . . .
C00R C 0.1964(2) -0.03445(13) 0.50802(11) 0.0177(3) Uani 1 1 d . . . . .
H00S H 0.143940 -0.087655 0.486619 0.021 Uiso 1 1 calc R . . . .
C00S C 0.2329(2) 0.40412(14) 0.30362(10) 0.0192(4) Uani 1 1 d . . . . .
H00T H 0.319096 0.371998 0.296098 0.029 Uiso 1 1 calc GR . . . .
H00U H 0.201828 0.449354 0.262442 0.029 Uiso 1 1 calc GR . . . .
H00V H 0.156001 0.358959 0.302828 0.029 Uiso 1 1 calc GR . . . .
C00T C 0.2925(2) -0.04008(12) 0.58024(11) 0.0188(4) Uani 1 1 d . . . . .
H00W H 0.307464 -0.097312 0.606952 0.023 Uiso 1 1 calc R . . . .
C00U C 0.0835(2) 0.06006(14) 0.38655(11) 0.0206(4) Uani 1 1 d . . . . .
H00X H 0.016886 0.111946 0.385238 0.031 Uiso 1 1 calc GR . . . .
H00Y H 0.028905 0.002791 0.372431 0.031 Uiso 1 1 calc GR . . . .
H H 0.144430 0.071617 0.350217 0.031 Uiso 1 1 calc GR . . . .


_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 Cl02 2.3300(4) . ?
Pd01 Cl03 2.3203(5) . ?
Pd01 N004 2.0269(14) . ?
Pd01 N005 2.0489(14) . ?
Pd01 C007 2.5038(16) . ?
N004 C008 1.360(2) . ?
N004 C00E 1.354(2) . ?
N005 C006 1.368(2) . ?
N005 C00L 1.351(2) . ?
C006 C00A 1.499(2) . ?
C006 C00H 1.391(2) . ?
C007 C009 1.322(2) . ?
C007 C00A 1.321(2) . ?
C008 C009 1.490(2) . ?
C008 C00P 1.391(2) . ?
C009 C00C 1.501(2) . ?
C00A C00F 1.548(2) . ?
C00B C00I 1.380(3) . ?
C00B C00L 1.395(2) . ?
C00C C00G 1.397(3) . ?
C00C C00K 1.399(2) . ?
C00D C00G 1.394(2) . ?
C00D C00N 1.393(3) . ?
C00E C00R 1.387(3) . ?
C00E C00U 1.499(2) . ?
C00F C00M 1.544(2) . ?
C00F C00O 1.540(2) . ?
C00F C00Q 1.536(2) . ?
C00H C00I 1.388(2) . ?
C00J C00K 1.392(3) . ?
C00J C00N 1.383(3) . ?
C00L C00S 1.501(2) . ?
C00P C00T 1.394(3) . ?
C00R C00T 1.382(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
Cl02 Pd01 C007 92.41(4) . . ?
Cl03 Pd01 Cl02 170.825(16) . . ?
Cl03 Pd01 C007 96.28(4) . . ?
N004 Pd01 Cl02 89.67(4) . . ?
N004 Pd01 Cl03 88.97(4) . . ?
N004 Pd01 N005 159.00(6) . . ?
N004 Pd01 C007 80.00(6) . . ?
N005 Pd01 Cl02 93.56(4) . . ?
N005 Pd01 Cl03 90.96(4) . . ?
N005 Pd01 C007 79.13(6) . . ?
C008 N004 Pd01 112.11(11) . . ?
C00E N004 Pd01 126.91(12) . . ?
C00E N004 C008 120.95(15) . . ?
C006 N005 Pd01 112.07(11) . . ?
C00L N005 Pd01 126.94(12) . . ?
C00L N005 C006 120.56(15) . . ?
N005 C006 C00A 117.94(14) . . ?
N005 C006 C00H 119.93(16) . . ?
C00H C006 C00A 122.12(15) . . ?
C009 C007 Pd01 94.04(11) . . ?
C00A C007 Pd01 93.57(11) . . ?
C00A C007 C009 172.31(17) . . ?
N004 C008 C009 119.37(14) . . ?
N004 C008 C00P 120.28(16) . . ?
C00P C008 C009 120.34(15) . . ?
C007 C009 C008 122.65(15) . . ?
C007 C009 C00C 118.68(15) . . ?
C008 C009 C00C 118.67(14) . . ?
C006 C00A C00F 120.87(14) . . ?
C007 C00A C006 119.48(16) . . ?
C007 C00A C00F 119.58(15) . . ?
C00I C00B C00L 119.70(17) . . ?
C00G C00C C009 120.17(15) . . ?
C00G C00C C00K 119.47(16) . . ?
C00K C00C C009 120.31(16) . . ?
C00N C00D C00G 119.95(18) . . ?
N004 C00E C00R 120.07(16) . . ?
N004 C00E C00U 116.92(16) . . ?
C00R C00E C00U 122.98(16) . . ?
C00M C00F C00A 109.21(14) . . ?
C00O C00F C00A 108.78(14) . . ?
C00O C00F C00M 109.02(14) . . ?
C00Q C00F C00A 111.28(14) . . ?
C00Q C00F C00M 110.67(14) . . ?
C00Q C00F C00O 107.83(15) . . ?
C00D C00G C00C 120.13(17) . . ?
C00I C00H C006 119.94(17) . . ?
C00B C00I C00H 119.27(16) . . ?
C00N C00J C00K 120.46(17) . . ?
C00J C00K C00C 119.91(17) . . ?
N005 C00L C00B 120.59(16) . . ?
N005 C00L C00S 118.07(15) . . ?
C00B C00L C00S 121.35(16) . . ?
C00J C00N C00D 120.02(17) . . ?
C008 C00P C00T 119.22(16) . . ?
C00T C00R C00E 120.12(17) . . ?
C00R C00T C00P 119.25(16) . . ?

_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 1.640
_oxdiff_exptl_absorpt_empirical_full_min 0.515
