π-Bonded Dithiolene Complexes: Synthesis, Molecular Structures, Electrochemical Behavior, and Density Functional Theory Calculations
Aurélie Damas; Lise-Marie Chamoreau; Andrew L. Cooksy; Anny Jutand; Hani Amouri; Inorganic Chemistry 52 (2013) 1409–1417; doi:10.1021/ic302128q

data_4333681
_publ_contact_author
;
  Hani Amouri
;
_publ_contact_author_email       hani.amouri@upmc.fr
_publ_contact_author_fax         '00 33 1 44 27 38 41'
_publ_contact_author_phone       '00 33 1 44 27 30 83'
_publ_section_title
;
 \p-Bonded Dithiolene Complexes: Synthesis, Molecular Structures,
 Electrochemical Behavior, and Density Functional Theory Calculations
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1409
_journal_page_last               1417
_journal_paper_doi               10.1021/ic302128q
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C16 H19 Ir S2, C H2 Cl2'
_chemical_formula_sum            'C17 H21 Cl2 Ir O0 S2'
_chemical_formula_weight         552.56
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.915(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.853(2)
_cell_length_b                   14.1687(12)
_cell_length_c                   17.017(3)
_cell_measurement_reflns_used    104
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      17.6
_cell_measurement_theta_min      3.1
_cell_volume                     3820.2(9)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.877
_diffrn_measured_fraction_theta_max 0.877
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0633
_diffrn_reflns_av_sigmaI/netI    0.0789
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            31807
_diffrn_reflns_theta_full        30.01
_diffrn_reflns_theta_max         30.01
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    7.482
_exptl_absorpt_correction_T_max  0.550
_exptl_absorpt_correction_T_min  0.199
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.921
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.08
_refine_diff_density_max         6.992
_refine_diff_density_min         -4.664
_refine_diff_density_rms         0.397
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.164
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     402
_refine_ls_number_reflns         9769
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.163
_refine_ls_R_factor_all          0.1551
_refine_ls_R_factor_gt           0.1038
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0163P)^2^+370.8189P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2408
_refine_ls_wR_factor_ref         0.2644
_reflns_number_gt                6524
_reflns_number_total             9769
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic302128q_si_002_2.cif
_cod_data_source_block           ad007
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4333681