#------------------------------------------------------------------------------
#$Date: 2023-12-08 19:12:05 +0200 (Fri, 08 Dec 2023) $
#$Revision: 288193 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/23/7702339.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7702339
loop_
_publ_author_name
'Arca, Massimiliano'
'Demartin, Francesco'
'Devillanova, Francesco A.'
'Garau, Alessandra'
'Isaia, Francesco'
'Lelj, Francesco'
'Lippolis, Vito'
'Pedraglio, Samuele'
'Verani, Gaetano'
_publ_section_title
;
 Synthesis, X-ray crystal structure and spectroscopic characterization of
 the new dithiolene [Pd(Et2timdt)2] and of its adduct with molecular
 diiodine [Pd(Et2timdt)2]·I2·CHCl3
 (Et2timdt = monoanion of
 1,3-diethylimidazolidine-2,4,5-trithione)
;
_journal_issue                   22
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3731
_journal_paper_doi               10.1039/a805494k
_journal_year                    1998
_chemical_formula_sum            'C15 H21 Cl3 I2 N4 Pd S6'
_chemical_formula_weight         916.31
_space_group_IT_number           6
_space_group_name_Hall           'P -2y'
_space_group_name_H-M_alt        'P 1 m 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 m 1'
_audit_creation_date             98-09-10
_audit_creation_method           'from The Personal SDP version 2.1.1'
_audit_update_record
;
 ?
;
_cell_angle_alpha                90.0000(0)
_cell_angle_beta                 102.83(4)
_cell_angle_gamma                90.0000(0)
_cell_formula_units_Z            4
_cell_length_a                   21.724(9)
_cell_length_b                   12.901(4)
_cell_length_c                   11.004(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      11
_cell_measurement_theta_min      8
_cell_volume                     3007(2)
_computing_cell_refinement       'CAD4 (Enraf Nonius)'
_computing_data_collection       'CAD4 (Enraf Nonius)'
_computing_data_reduction        'The Personal SDP, 1991'
_computing_molecular_graphics    'The Personal SDP (1991)'
_computing_publication_material  'The Personal SDP (1991)'
_computing_structure_refinement
' Full-matrix least-squares  (The Personal SDP, 1991)'
_computing_structure_solution
' SIR  (G. Cascarano and C. Giacovazzo, 1988) as implemented in The Personal SDP'
_diffrn_ambient_temperature      293
_diffrn_measurement_device       'CAD4 (Enraf Nonius)'
_diffrn_measurement_method       omega
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2970
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.00
_diffrn_standards_decay_%        10.64
_diffrn_standards_interval_time  173
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    332.55
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.683
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
' The correction was based on a series of psi-scans.'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    2.024
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.318
_refine_diff_density_min         -.645
_refine_ls_extinction_coef       0.0000
_refine_ls_extinction_method     'secondary Zachariasen'
_refine_ls_goodness_of_fit_all   1.254
_refine_ls_goodness_of_fit_obs   1.913
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    27
_refine_ls_number_parameters     181
_refine_ls_number_reflns         1272
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.304
_refine_ls_R_factor_obs          0.053
_refine_ls_shift/esd_max         0.454
_refine_ls_shift/esd_mean        0.040
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.064
_reflns_limit_h_max              25
_reflns_limit_h_min              -25
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              13
_reflns_limit_l_min              0
_reflns_number_observed          1303
_reflns_number_total             2757
_reflns_observed_criterion
' refln observed if F~o~ > 2.0 * 3.00 * sigma(F~o~)'
_cod_data_source_file            805494k.txt
_cod_data_source_block           compound_6
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '_exptl_abosrpt_process_details' was replaced with
'_exptl_absorpt_process_details' as specified in the replacement file
'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_cell_volume        3007.0(22)
_cod_original_sg_symbol_H-M      'C 1 2/m 1'
_cod_database_code               7702339
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
+x,-y,+z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_type_symbol
I1 0.92324(9) 0.0000(0) 0.5705(2) 0.50 0.179(1) Uani I
I2 0.81680(7) 0.0000(0) 0.6764(1) 0.50 0.0879(7) Uani I
PD 0.49156(6) 0.0000(0) 0.2345(1) 0.50 0.0559(5) Uani PD
S1a 0.5397(1) 0.1286(3) 0.3646(3) 1.00 0.061(2) Uani S
S2a 0.7074(3) 0.0000(0) 0.7830(5) 0.50 0.075(3) Uani S
N1a 0.6247(4) 0.0842(8) 0.5843(8) 1.00 0.058(5) Uani N
C1a 0.5830(5) 0.0521(9) 0.4772(9) 1.00 0.057(5) Uani C
C2a 0.6498(8) 0.0000(0) 0.645(2) 0.50 0.064(7) Uani C
C3a 0.6355(6) 0.195(1) 0.626(1) 1.00 0.077(8) Uani C
C4a 0.6849(7) 0.237(1) 0.569(1) 1.00 0.096(9) Uani C
S1b 0.4437(1) 0.1276(3) 0.1025(3) 1.00 0.063(2) Uani S
S2b 0.2915(2) 0.0000(0) -0.3307(5) 0.50 0.077(2) Uani S
N1b 0.3659(4) 0.0845(8) -0.1237(8) 1.00 0.056(4) Uani N
C1b 0.4024(5) 0.0544(9) -0.0149(9) 1.00 0.063(5) Uani C
C2b 0.3413(7) 0.0000(0) -0.196(1) 0.50 0.046(7) Uani C
C3b 0.3511(6) 0.193(1) -0.160(1) 1.00 0.073(6) Uani C
C4b 0.2986(7) 0.232(1) -0.102(1) 1.00 0.107(8) Uani C
CL1s 0.4257(7) 0.3917(9) 0.145(2) 0.60 0.22(1) Uani CL
CL2s 0.336(1) 0.5000(0) 0.138(3) 0.30 0.53(2) Uani CL
CS 0.414(2) 0.5000(0) 0.157(8) 0.30 0.25(5) Uani C
H3a1 0.6486(0) 0.1984(0) 0.7138(0) 1.00 0.1027(0) Uiso H
H3b1 0.3382(0) 0.1971(0) -0.2483(0) 1.00 0.0813(0) Uiso H
H3b2 0.3876(0) 0.2343(0) -0.1323(0) 1.00 0.0813(0) Uiso H
H3a2 0.5977(0) 0.2339(0) 0.5991(0) 1.00 0.1027(0) Uiso H
H4b1 0.2893(0) 0.3018(0) -0.1262(0) 1.00 0.1177(0) Uiso H
H4a1 0.6929(0) 0.3070(0) 0.5929(0) 1.00 0.1268(0) Uiso H
H4b2 0.2620(0) 0.1904(0) -0.1301(0) 1.00 0.1177(0) Uiso H
H4a2 0.7225(0) 0.1974(0) 0.5952(0) 1.00 0.1268(0) Uiso H
H4a3 0.6716(0) 0.2329(0) 0.4804(0) 1.00 0.1268(0) Uiso H
H4b3 0.3115(0) 0.2276(0) -0.0141(0) 1.00 0.1177(0) Uiso H
loop_
_atom_type_symbol
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
I 0 8 -.7260 1.8120 'International Tables Vol IV Table 2.2A'
PD 0 4 -1.177 1.0070 'International Tables Vol IV Table 2.2A'
CL 0 12 0.1320 0.1590 'International Tables Vol IV Table 2.2A'
S 0 24 0.1100 0.1240 'International Tables Vol IV Table 2.2A'
N 0 16 0.0040 0.0030 'International Tables Vol IV Table 2.2A'
C 0 60 0.0020 0.0020 'International Tables Vol IV Table 2.2A'
H 0 84 0.0000 0.0000 'International Tables Vol IV Table 2.2A'
loop_
_diffrn_attenuator_code
_diffrn_attenuator_scale
1 17.023
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
-8 0 0
9 -3 0
9 3 0
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S1a PD S1a 93.0(1) 1_555 1_555 2_555 yes
S1a PD S1b 87.4(1) 1_555 1_555 1_555 yes
S1a PD S1b 179.3(1) 1_555 1_555 2_555 yes
S1a PD S1b 179.3(1) 2_555 1_555 1_555 yes
S1a PD S1b 87.4(1) 2_555 1_555 2_555 yes
S1b PD S1b 92.1(1) 1_555 1_555 2_555 yes
PD S1a C1a 97.9(4) 1_555 1_555 1_555 yes
C1a N1a C2a 107.5(10) 1_555 1_555 1_555 yes
C1a N1a C3a 124.9(10) 1_555 1_555 1_555 yes
C2a N1a C3a 127.4(9) 1_555 1_555 1_555 yes
S1a C1a N1a 126.9(9) 1_555 1_555 1_555 yes
S1a C1a C1a 125.6(8) 1_555 1_555 2_555 yes
N1a C1a C1a 107.5(9) 1_555 1_555 2_555 yes
S2a C2a N1a 125.0(7) 1_555 1_555 1_555 yes
S2a C2a N1a 125.0(7) 1_555 1_555 2_555 yes
N1a C2a N1a 109.9(12) 1_555 1_555 2_555 yes
N1a C3a C4a 107.5(12) 1_555 1_555 1_555 yes
N1a C3a H3a1 110.0(13) 1_555 1_555 1_555 yes
N1a C3a H3a2 110.0(11) 1_555 1_555 1_555 yes
C4a C3a H3a1 110.0(12) 1_555 1_555 1_555 yes
C4a C3a H3a2 110.0(14) 1_555 1_555 1_555 yes
H3a1 C3a H3a2 109.5(15) 1_555 1_555 1_555 yes
C3a C4a H4a1 109.5(15) 1_555 1_555 1_555 yes
C3a C4a H4a2 109.5(15) 1_555 1_555 1_555 yes
C3a C4a H4a3 109.5(13) 1_555 1_555 1_555 yes
H4a1 C4a H4a2 109.5(14) 1_555 1_555 1_555 yes
H4a1 C4a H4a3 109.5(16) 1_555 1_555 1_555 yes
H4a2 C4a H4a3 109.5(16) 1_555 1_555 1_555 yes
PD S1b C1b 99.9(4) 1_555 1_555 1_555 yes
C1b N1b C2b 111.3(10) 1_555 1_555 1_555 yes
C1b N1b C3b 124.8(9) 1_555 1_555 1_555 yes
C2b N1b C3b 123.9(8) 1_555 1_555 1_555 yes
S1b C1b N1b 129.1(9) 1_555 1_555 1_555 yes
S1b C1b C1b 124.0(8) 1_555 1_555 2_555 yes
N1b C1b C1b 106.9(9) 1_555 1_555 2_555 yes
S2b C2b N1b 128.1(6) 1_555 1_555 1_555 yes
S2b C2b N1b 128.1(6) 1_555 1_555 2_555 yes
N1b C2b N1b 103.6(10) 1_555 1_555 2_555 yes
N1b C3b C4b 109.9(11) 1_555 1_555 1_555 yes
N1b C3b H3b1 109.4(12) 1_555 1_555 1_555 yes
N1b C3b H3b2 109.4(11) 1_555 1_555 1_555 yes
C4b C3b H3b1 109.4(11) 1_555 1_555 1_555 yes
C4b C3b H3b2 109.4(12) 1_555 1_555 1_555 yes
H3b1 C3b H3b2 109.5(14) 1_555 1_555 1_555 yes
C3b C4b H4b1 109.5(14) 1_555 1_555 1_555 yes
C3b C4b H4b2 109.5(14) 1_555 1_555 1_555 yes
C3b C4b H4b3 109.5(12) 1_555 1_555 1_555 yes
H4b1 C4b H4b2 109.5(13) 1_555 1_555 1_555 yes
H4b1 C4b H4b3 109.5(16) 1_555 1_555 1_555 yes
H4b2 C4b H4b3 109.5(16) 1_555 1_555 1_555 yes
CL1s CS CL1s 154.1(54) 1_555 1_555 2_565 yes
CL1s CS CL2s 101.0(15) 1_555 1_555 1_555 yes
CL1s CS CL2s 101.0(15) 2_565 1_555 1_555 yes
I1 I1 I2 178.5(1) *_756 1_555 1_555 yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I2 S2a 2.875(6) 1_555 1_555 yes
I2 S2a 2.875(6) 1_555 2_555 yes
I2 S2b 4.004(5) 1_555 *_655 yes
I2 S2b 4.004(5) 1_555 *_655 yes
PD S1a 2.287(3) 1_555 1_555 yes
PD S1a 2.287(3) 1_555 2_555 yes
PD S1b 2.286(3) 1_555 1_555 yes
PD S1b 2.286(3) 1_555 2_555 yes
S1a C1a 1.697(11) 1_555 1_555 yes
S2a C2a 1.740(16) 1_555 1_555 yes
S2a C2a 1.740(16) 1_555 2_555 yes
N1a C1a 1.382(13) 1_555 1_555 yes
N1a C2a 1.327(13) 1_555 1_555 yes
N1a C2a 1.327(13) 1_555 2_555 yes
N1a C3a 1.504(18) 1_555 1_555 yes
C1a C1a 1.343(17) 1_555 2_555 yes
C3a C4a 1.460(22) 1_555 1_555 yes
C3a H3a1 0.950(14) 1_555 1_555 yes
C3a H3a2 0.950(14) 1_555 1_555 yes
C4a H4a1 0.950(18) 1_555 1_555 yes
C4a H4a2 0.950(15) 1_555 1_555 yes
C4a H4a3 0.950(14) 1_555 1_555 yes
S1b C1b 1.689(11) 1_555 1_555 yes
S2b C2b 1.626(14) 1_555 1_555 yes
S2b C2b 1.626(14) 1_555 2_555 yes
N1b C1b 1.339(12) 1_555 1_555 yes
N1b C2b 1.388(13) 1_555 1_555 yes
N1b C2b 1.388(13) 1_555 2_555 yes
N1b C3b 1.469(17) 1_555 1_555 yes
C1b C1b 1.403(17) 1_555 2_555 yes
C3b C4b 1.510(21) 1_555 1_555 yes
C3b H3b1 0.950(12) 1_555 1_555 yes
C3b H3b2 0.950(13) 1_555 1_555 yes
C4b H4b1 0.950(17) 1_555 1_555 yes
C4b H4b2 0.950(15) 1_555 1_555 yes
C4b H4b3 0.950(14) 1_555 1_555 yes
CL1s CS 1.433(19) 1_555 1_555 yes
CL1s CS 1.433(19) 1_555 2_565 yes
CL2s CS 1.654(46) 1_555 1_555 yes
CL2s CS 1.654(46) 1_555 2_565 yes
I1 I1 3.978(3) 1_555 *_756 yes
I1 I1 3.978(3) 1_555 *_756 yes
I1 I2 2.811(3) 1_555 1_555 yes
I1 I2 2.811(3) 1_555 2_555 yes
loop_
_reflns_scale_group_code
_reflns_scale_meas_F
1 1.786517
