Intriguing I2 Reduction in the Iodide for Chloride Ligand Substitution at a Ru(II) Complex: Role of Mixed Trihalides in the Redox Mechanism.
Mosquera, Marta E. G.; Gomez-Sal, Pilar; Diaz, Isabel; Aguirre, Lina M.; Ienco, A.; Manca, Gabriele; Mealli, Carlo; Inorganic chemistry 55 (2015) 283–; doi:10.1021/acs.inorgchem.5b02307

data_4344847
_publ_section_title
;
 Intriguing I2 Reduction in the Iodide for Chloride Ligand Substitution at
 a Ru(II) Complex: Role of Mixed Trihalides in the Redox Mechanism.
;
_journal_issue                   1
_journal_name_full               'Inorganic chemistry'
_journal_page_first              283
_journal_paper_doi               10.1021/acs.inorgchem.5b02307
_journal_volume                  55
_journal_year                    2015
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C20 H36 Cl1 I7 N4 Ru1'
_chemical_formula_sum            'C20 H36 Cl I7 N4 Ru'
_chemical_formula_weight         1357.35
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      62
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2014-07-04T12:00:45-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.735(3)
_cell_length_b                   14.945(2)
_cell_length_c                   11.6353(12)
_cell_measurement_reflns_used    231
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      16.23
_cell_measurement_theta_min      3.46
_cell_measurement_wavelength     0.71073
_cell_volume                     3953.4(8)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_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)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_UB_11      0.01
_diffrn_orient_matrix_UB_12      0
_diffrn_orient_matrix_UB_13      0
_diffrn_orient_matrix_UB_21      0
_diffrn_orient_matrix_UB_22      0.01
_diffrn_orient_matrix_UB_23      0
_diffrn_orient_matrix_UB_31      0
_diffrn_orient_matrix_UB_32      0
_diffrn_orient_matrix_UB_33      0.01
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1114
_diffrn_reflns_av_unetI/netI     0.1737
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            18577
_diffrn_reflns_reduction_process
;
 Scaled and merged with Sortav
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        25.31
_diffrn_reflns_theta_max         25.31
_diffrn_reflns_theta_min         3.21
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    5.945
_exptl_absorpt_correction_T_max  0.083
_exptl_absorpt_correction_T_min  0.042
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.281
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2464
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.27
_refine_diff_density_max         3.349
_refine_diff_density_min         -3.336
_refine_diff_density_rms         0.355
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.938
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         3683
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.938
_refine_ls_R_factor_all          0.159
_refine_ls_R_factor_gt           0.1302
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0751P)^2^+566.7947P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3223
_refine_ls_wR_factor_ref         0.3422
_reflns_number_gt                2560
_reflns_number_total             3683
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic5b02307_si_001.cif
_cod_data_source_block           3.3I2
_cod_database_code               4344847