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)
Arca, Massimiliano; Demartin, Francesco; Devillanova, Francesco A.; Garau, Alessandra; Isaia, Francesco; Lelj, Francesco; Lippolis, Vito; Pedraglio, Samuele; Verani, Gaetano; Journal of the Chemical Society, Dalton Transactions  (1998) 3731–; doi:10.1039/a805494k

data_7702339
_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]&#x00B7;I2&#x00B7;CHCl3
 (Et2timdt&#x2005;=&#x2005;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