Redox Activity of Oxo-Bridged Iridium Dimers in an N,O-Donor Environment: Characterization of Remarkably Stable Ir(IV,V) Complexes.
Sinha, Shashi Bhushan; Shopov, Dimitar Y.; Sharninghausen, Liam S.; Stein, Christopher J.; Mercado, Brandon Q.; Balcells, David; Pedersen, Thomas Bondo; Reiher, Markus; Brudvig, Gary W.; Crabtree, Robert H.; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b04874

data_4126263
_publ_section_title
;
 Redox Activity of Oxo-Bridged Iridium Dimers in an N,O-Donor Environment:
 Characterization of Remarkably Stable Ir(IV,V) Complexes.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b04874
_journal_year                    2017
_chemical_formula_moiety         'C32 H42 Cl2 Ir2 N4 O5, 2(C H2 Cl2), H2 O'
_chemical_formula_sum            'C34 H48 Cl6 Ir2 N4 O6'
_chemical_formula_weight         1205.86
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     SHELXT
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                78.986(3)
_cell_angle_beta                 81.048(3)
_cell_angle_gamma                66.372(4)
_cell_formula_units_Z            2
_cell_length_a                   11.0784(5)
_cell_length_b                   11.9210(5)
_cell_length_c                   17.2179(6)
_cell_measurement_reflns_used    40691
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      66.6190
_cell_measurement_theta_min      2.5890
_cell_volume                     2036.98(16)
_computing_cell_refinement       'CrysAlisPro 1.171.39.16b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.16b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.16b (Rigaku OD, 2015)'
_computing_molecular_graphics
; 
Dolomanov, O.V.; Bourhis, L.J.; Gildea, R.J.; Howard, J.A.K.; Puschmann, H., 
OLEX2: A complete structure solution, refinement and analysis program 
(2009). J. Appl. Cryst., 42, 339-341. 
;
_computing_publication_material  'CIFTAB-2014/2 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 22.2
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Rigaku Saturn 944+ CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_unetI/netI     0.0184
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            74262
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        66.869
_diffrn_reflns_theta_max         66.869
_diffrn_reflns_theta_min         2.625
_diffrn_source                   'microfocus rotating anode'
_exptl_absorpt_coefficient_mu    16.480
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41620
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.39.16b (Rigaku Oxford Diffraction, 2015) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.966
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.725
_refine_diff_density_min         -1.329
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         7095
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0215
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0292P)^2^+3.5152P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0523
_refine_ls_wR_factor_ref         0.0542
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6553
_reflns_number_total             7095
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b04874_si_003.cif
_cod_data_source_block           007-16070
_cod_database_code               4126263
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.290
_shelx_estimated_absorpt_t_max   0.734
_shelx_res_checksum              48783
_shelx_hkl_checksum              18513