Stable Iridium(IV) Complexes of an Oxidation-Resistant Pyridine-Alkoxide Ligand: Highly Divergent Redox Properties Depending on the Isomeric Form Adopted.
Shopov, Dimitar Y.; Rudshteyn, Benjamin; Campos, Jesús; Batista, Victor S.; Crabtree, Robert H.; Brudvig, Gary W.; Journal of the American Chemical Society 137 (2015) 7243–7250; doi:10.1021/jacs.5b04185

data_4123768
_publ_contact_author
;
 Dr. Robert H. Crabtree           
 The Department of Chemistry 
 Yale University 
 P. O. Box 208107 
 New Haven 
 Connecticut 06520 USA.
;
_publ_section_title
;
 Stable Iridium(IV) Complexes of an Oxidation-Resistant Pyridine-Alkoxide
 Ligand: Highly Divergent Redox Properties Depending on the Isomeric Form
 Adopted.
;
_journal_issue                   22
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7243
_journal_page_last               7250
_journal_paper_doi               10.1021/jacs.5b04185
_journal_volume                  137
_journal_year                    2015
_chemical_formula_sum            'C55 H84 Cl4 Ir2 Mg N6 O14'
_chemical_formula_weight         1603.79
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                66.875(5)
_cell_angle_beta                 71.497(5)
_cell_angle_gamma                68.005(5)
_cell_formula_units_Z            1
_cell_length_a                   11.4260(6)
_cell_length_b                   12.5211(5)
_cell_length_c                   14.2417(10)
_cell_measurement_reflns_used    39442
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     1702.42(18)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r12 '
_computing_data_collection       'CrystalClear-SM Expert 2.0 r12 '
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r12 '
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
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_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID imaging plate'
_diffrn_measurement_method       \w
_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  0.0848
_diffrn_reflns_av_sigmaI/netI    0.0504
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            55494
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    4.131
_exptl_absorpt_correction_T_max  0.6370
_exptl_absorpt_correction_T_min  0.5762
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private Communication'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             802
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
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_platon_squeeze_details
;
The unit cell contains 2 acetone molecules and one dichloromethane molecule 
which have been treated as a diffuse contribution to the overall scattering 
without specific atom positions by SQUEEZE/PLATON. These solvent molecules
are allocated in a long accesible void of 462 A3. 
;
_refine_diff_density_max         2.134
_refine_diff_density_min         -2.166
_refine_diff_density_rms         0.202
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         7787
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0535
_refine_ls_R_factor_gt           0.0425
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0585P)^2^+10.4759P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0952
_refine_ls_wR_factor_ref         0.1155
_reflns_number_gt                6789
_reflns_number_total             7787
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5b04185_si_004.cif
_cod_data_source_block           14028
_cod_depositor_comments
'Adding full bibliography for 4123768--4123770.cif.'
_cod_original_cell_volume        1702.42(16)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4123768