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_4333680
_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
'2(C26 H34 Ir2 S2)2-, 4(C F3 S O3)-, (C4 H10 O), (H2O)'
_chemical_formula_sum            'C30 H40 F6 Ir2 O7 S4'
_chemical_formula_weight         1139.26
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      1
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                101.871(16)
_cell_angle_beta                 99.168(10)
_cell_angle_gamma                97.776(12)
_cell_formula_units_Z            2
_cell_length_a                   8.9356(10)
_cell_length_b                   12.2850(19)
_cell_length_c                   18.6118(17)
_cell_measurement_reflns_used    153
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      22.1
_cell_measurement_theta_min      3
_cell_volume                     1943.8(4)
_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    'Ortep-3 for Windows (Farrugia, 1997)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0504
_diffrn_reflns_av_sigmaI/netI    0.0877
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            49814
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.87
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.124
_exptl_absorpt_correction_T_max  0.457
_exptl_absorpt_correction_T_min  0.232
_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    1.947
_exptl_crystal_description       needle
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.73
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.419
_refine_diff_density_min         -2.111
_refine_diff_density_rms         0.209
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.543(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     871
_refine_ls_number_reflns         21600
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0396P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.0858
_reflns_number_gt                16747
_reflns_number_total             21600
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic302128q_si_002_1.cif
_cod_data_source_block           ad029
_cod_database_code               4333680