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_4130875
_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_absolute_configuration ad
_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      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 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                90
_cell_angle_beta                 102.709(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   33.1646(12)
_cell_length_b                   16.8051(5)
_cell_length_c                   16.1160(4)
_cell_measurement_reflns_used    24031
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      66.4870
_cell_measurement_theta_min      2.7120
_cell_volume                     8761.9(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41o (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41o (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41o (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-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 22.2
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku Saturn 944+ CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'microfocus rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1609
_diffrn_reflns_av_unetI/netI     0.1025
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            103746
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        66.964
_diffrn_reflns_theta_max         66.964
_diffrn_reflns_theta_min         2.732
_exptl_absorpt_coefficient_mu    13.001
_exptl_absorpt_correction_T_max  1.461
_exptl_absorpt_correction_T_min  0.717
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Empirical correction (ABSPACK)'
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Shard
_exptl_crystal_F_000             3904
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_refine_diff_density_max         2.323
_refine_diff_density_min         -3.667
_refine_diff_density_rms         0.210
_refine_ls_abs_structure_details
; 
 Flack x determined using 4532 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.03(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     827
_refine_ls_number_reflns         15122
_refine_ls_number_restraints     908
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0896
_refine_ls_R_factor_gt           0.0721
_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^)+(0.1044P)^2^+49.0252P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1705
_refine_ls_wR_factor_ref         0.1844
_reflns_Friedel_coverage         0.945
_reflns_Friedel_fraction_full    0.942
_reflns_Friedel_fraction_max     0.942
_reflns_number_gt                12164
_reflns_number_total             15122
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b07716_si_003.cif
_cod_data_source_block           007-16107
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               4130875
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.563
_shelx_estimated_absorpt_t_max   0.781
_shelx_res_checksum              69300
_shelx_hkl_checksum              39495
_shelx_fab_checksum              59284