# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2020

####################################################################### 
# 
# 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_[Pd(MeImHS)4]I4
_database_code_depnum_ccdc_archive 'CCDC 1964288'
loop_
_audit_author_name
_audit_author_address
'Francesco Demartin'
;Universita degli Studi di Milano Dipartimento di Chimica
Italy
;
_audit_update_record             
;
2019-11-07 deposited with the CCDC.	2020-01-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H24 I3.46 N8 Pd S4'
_chemical_formula_weight         1002.14

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   8.7210(17)
_cell_length_b                   12.844(3)
_cell_length_c                   14.190(3)
_cell_angle_alpha                90
_cell_angle_beta                 99.62(3)
_cell_angle_gamma                90
_cell_volume                     1567.1(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    294(2)
_cell_measurement_reflns_used    5757
_cell_measurement_theta_min      2.56
_cell_measurement_theta_max      24.90

_exptl_crystal_description       prism
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.124
_exptl_crystal_F_000             939
_exptl_transmission_factor_min   0.842
_exptl_transmission_factor_max   1.000
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_exptl_absorpt_coefficient_mu    4.287
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      294(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'APEX II CCD diffractometer'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10812
_diffrn_reflns_av_unetI/netI     0.0216
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.152
_diffrn_reflns_theta_max         25.274
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             2824
_reflns_number_gt                2273
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0704P)²+11.1450P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2824
_refine_ls_number_parameters     160
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0478
_refine_ls_wR_factor_ref         0.1476
_refine_ls_wR_factor_gt          0.1393
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_restrained_S_all      1.095
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd Pd 0.000000 0.000000 0.000000 0.0361(3) Uani 1 2 d S . P . .
I2 I 0.1419(4) 0.2705(4) -0.4943(4) 0.0553(6) Uani 0.73 1 d . . P . .
I1 I 0.39866(11) 0.08395(9) -0.50169(7) 0.0666(3) Uani 0.73 1 d . . P . .
S2 S -0.0101(3) -0.04800(17) -0.15955(14) 0.0451(5) Uani 1 1 d . . . . .
S1 S -0.2190(3) -0.1042(2) -0.00748(18) 0.0616(7) Uani 1 1 d . . . . .
N3 N -0.1790(9) 0.1342(7) -0.1861(5) 0.0532(19) Uani 1 1 d . . . . .
H3 H -0.200274 0.137737 -0.129136 0.064 Uiso 1 1 calc R U . . .
N4 N -0.0884(9) 0.0820(6) -0.3101(5) 0.0445(17) Uani 1 1 d . . . . .
N2 N -0.2906(10) -0.1582(7) 0.1673(6) 0.062(2) Uani 1 1 d . . . . .
C5 C -0.0957(10) 0.0590(7) -0.2178(6) 0.0396(18) Uani 1 1 d . . . . .
N1 N -0.3801(11) -0.0109(7) 0.1176(6) 0.064(2) Uani 1 1 d . . . . .
H1 H -0.400501 0.043532 0.082520 0.077 Uiso 1 1 calc R U . . .
C7 C -0.1679(13) 0.1723(9) -0.3335(7) 0.065(3) Uani 1 1 d . . . . .
H7 H -0.179523 0.205467 -0.392565 0.078 Uiso 1 1 calc R U . . .
C6 C -0.2261(14) 0.2053(9) -0.2575(8) 0.068(3) Uani 1 1 d . . . . .
H6 H -0.286368 0.264344 -0.253657 0.081 Uiso 1 1 calc R U . . .
C8 C -0.0017(15) 0.0207(8) -0.3697(7) 0.063(3) Uani 1 1 d . . . . .
H8A H 0.097230 0.001551 -0.333328 0.075 Uiso 1 1 calc R U . . .
H8B H 0.014188 0.061111 -0.424118 0.075 Uiso 1 1 calc R U . . .
H8C H -0.059285 -0.041103 -0.390878 0.075 Uiso 1 1 calc R U . . .
C1 C -0.2954(11) -0.0907(8) 0.0967(6) 0.051(2) Uani 1 1 d . . . . .
C2 C -0.4303(16) -0.0268(15) 0.2020(10) 0.089(4) Uani 1 1 d . . . . .
H2 H -0.490631 0.017890 0.232213 0.106 Uiso 1 1 calc R U . . .
C3 C -0.3741(16) -0.1211(13) 0.2329(8) 0.081(4) Uani 1 1 d . . . . .
H3A H -0.389736 -0.154472 0.288690 0.098 Uiso 1 1 calc R U . . .
C4 C -0.215(2) -0.2606(10) 0.1724(11) 0.097(5) Uani 1 1 d . . . . .
H4A H -0.168859 -0.271150 0.116434 0.116 Uiso 1 1 calc R U . . .
H4B H -0.291680 -0.313795 0.175768 0.116 Uiso 1 1 calc R U . . .
H4C H -0.136622 -0.263914 0.228285 0.116 Uiso 1 1 calc R U . . .
I2' I 0.1809(12) 0.2577(9) -0.4891(8) 0.070(2) Uani 0.27 1 d . . P . .


_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
Pd S1 2.320(2) . ?
Pd S1 2.320(2) 3 ?
Pd S2 2.334(2) . ?
Pd S2 2.334(2) 3 ?
I1 I1 2.784(2) 3_654 ?
I1 I2' 2.955(10) . ?
S2 C5 1.710(9) . ?
S1 C1 1.728(9) . ?
N3 C5 1.330(12) . ?
N3 C6 1.375(13) . ?
N3 H3 0.8600 . ?
N4 C5 1.354(10) . ?
N4 C7 1.364(13) . ?
N4 C8 1.457(12) . ?
N2 C1 1.321(12) . ?
N2 C3 1.361(15) . ?
N2 C4 1.465(17) . ?
N1 C1 1.326(13) . ?
N1 C2 1.357(15) . ?
N1 H1 0.8600 . ?
C7 C6 1.335(16) . ?
C7 H7 0.9300 . ?
C6 H6 0.9300 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C2 C3 1.35(2) . ?
C2 H2 0.9300 . ?
C3 H3A 0.9300 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S1 Pd S1 180.0 . 3 ?
S1 Pd S2 84.61(9) . . ?
S1 Pd S2 95.39(9) 3 . ?
S1 Pd S2 95.39(9) . 3 ?
S1 Pd S2 84.61(9) 3 3 ?
S2 Pd S2 180.0 . 3 ?
I1 I1 I2' 175.3(2) 3_654 . ?
C5 S2 Pd 101.5(3) . . ?
C1 S1 Pd 109.6(3) . . ?
C5 N3 C6 110.2(8) . . ?
C5 N3 H3 124.9 . . ?
C6 N3 H3 124.9 . . ?
C5 N4 C7 108.5(8) . . ?
C5 N4 C8 123.8(8) . . ?
C7 N4 C8 127.6(8) . . ?
C1 N2 C3 109.6(11) . . ?
C1 N2 C4 125.7(11) . . ?
C3 N2 C4 124.5(12) . . ?
N3 C5 N4 106.6(8) . . ?
N3 C5 S2 129.7(6) . . ?
N4 C5 S2 123.7(7) . . ?
C1 N1 C2 110.9(11) . . ?
C1 N1 H1 124.6 . . ?
C2 N1 H1 124.6 . . ?
C6 C7 N4 108.6(8) . . ?
C6 C7 H7 125.7 . . ?
N4 C7 H7 125.7 . . ?
C7 C6 N3 106.1(9) . . ?
C7 C6 H6 126.9 . . ?
N3 C6 H6 126.9 . . ?
N4 C8 H8A 109.5 . . ?
N4 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N4 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C1 N1 106.6(9) . . ?
N2 C1 S1 128.0(9) . . ?
N1 C1 S1 125.3(8) . . ?
C3 C2 N1 105.5(12) . . ?
C3 C2 H2 127.2 . . ?
N1 C2 H2 127.2 . . ?
C2 C3 N2 107.4(11) . . ?
C2 C3 H3A 126.3 . . ?
N2 C3 H3A 126.3 . . ?
N2 C4 H4A 109.5 . . ?
N2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?

_refine_diff_density_max         1.666
_refine_diff_density_min         -1.091
_refine_diff_density_rms         0.158

