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_4130876
_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      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/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                 98.991(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.2543(15)
_cell_length_b                   8.3385(6)
_cell_length_c                   18.2152(12)
_cell_measurement_reflns_used    6372
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      67.0950
_cell_measurement_theta_min      3.9500
_cell_volume                     3338.6(4)
_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  'SHELXL-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 0.977
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1533
_diffrn_reflns_av_unetI/netI     0.0704
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            27605
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.907
_diffrn_reflns_theta_min         4.022
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    17.060
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69398
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.38.41o (Rigaku Oxford Diffraction, 2015) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.021
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         3.317
_refine_diff_density_min         -3.487
_refine_diff_density_rms         0.427
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.180
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         2956
_refine_ls_number_restraints     225
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.1204
_refine_ls_R_factor_gt           0.0874
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1090P)^2^+414.9259P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2241
_refine_ls_wR_factor_ref         0.2620
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2261
_reflns_number_total             2956
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b07716_si_002.cif
_cod_data_source_block           007-16008-2
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4130876
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              48644
_shelx_hkl_checksum              10471