High Oxidation State Iridium Mono-μ-oxo Dimers Related to Water Oxidation Catalysis.
Sharninghausen, Liam S.; Sinha, Shashi Bhushan; Shopov, Dimitar Y.; Choi, Bonnie; Mercado, Brandon Q.; Roy, Xavier; Balcells, David; Brudvig, Gary W.; Crabtree, Robert H.; Journal of the American Chemical Society 138 (2016) 15917–15926; doi:10.1021/jacs.6b07716

data_4130877
_publ_section_title
;
 High Oxidation State Iridium Mono-\m-oxo Dimers Related to Water
 Oxidation Catalysis.
;
_journal_issue                   49
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15917
_journal_page_last               15926
_journal_paper_doi               10.1021/jacs.6b07716
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C32 H40 Cl2 Ir2 N4 O5'
_chemical_formula_sum            'C32 H40 Cl2 Ir2 N4 O5'
_chemical_formula_weight         1015.98
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                69.8330(10)
_cell_angle_beta                 89.7210(10)
_cell_angle_gamma                67.8880(10)
_cell_formula_units_Z            2
_cell_length_a                   10.8298(8)
_cell_length_b                   12.6652(9)
_cell_length_c                   15.9733(11)
_cell_measurement_reflns_used    809
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.4
_cell_volume                     1885.6(2)
_computing_cell_refinement
'CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)'
_computing_data_reduction
'CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)'
_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-2013/2 (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 10
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID imaging plate'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0806
_diffrn_reflns_av_unetI/netI     0.0394
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_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       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            60758
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.495
_diffrn_reflns_theta_min         2.689
_diffrn_source                   'Sealed Tube'
_exptl_absorpt_coefficient_mu    7.233
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.614
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private Communication'
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.789
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.050
_refine_diff_density_max         2.721
_refine_diff_density_min         -0.736
_refine_diff_density_rms         0.190
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.961
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         8620
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.961
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0280
_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^)+(0.0452P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0693
_refine_ls_wR_factor_ref         0.0708
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7272
_reflns_number_total             8620
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b07716_si_004.cif
_cod_data_source_block           spider-16008
_cod_database_code               4130877
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.356
_shelx_estimated_absorpt_t_max   0.714
_shelx_res_checksum              78886
_shelx_hkl_checksum              66920
_shelx_fab_checksum              15819