New Ir Bis-Carbonyl Precursor for Water Oxidation Catalysis.
Huang, Daria L.; Beltrán-Suito, Rodrigo; Thomsen, Julianne M.; Hashmi, Sara M.; Materna, Kelly L.; Sheehan, Stafford W.; Mercado, Brandon Q.; Brudvig, Gary W.; Crabtree, Robert H.; Inorganic chemistry 55 (2016) 2427–2435; doi:10.1021/acs.inorgchem.5b02809

data_4347153
_publ_section_title
;
 New Ir Bis-Carbonyl Precursor for Water Oxidation Catalysis.
;
_journal_issue                   5
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2427
_journal_page_last               2435
_journal_paper_doi               10.1021/acs.inorgchem.5b02809
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C10 H10 Ir N O3, 0.5(C4 H10 O2)'
_chemical_formula_sum            'C12 H15 Ir N O4'
_chemical_formula_weight         429.45
_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   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                97.700(7)
_cell_angle_beta                 108.239(8)
_cell_angle_gamma                90.640(6)
_cell_formula_units_Z            2
_cell_length_a                   8.2220(2)
_cell_length_b                   8.8397(3)
_cell_length_c                   9.5097(7)
_cell_measurement_reflns_used    18890
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     649.49(6)
_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  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID imaging plate'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_av_unetI/netI     0.0142
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            19760
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.470
_diffrn_reflns_theta_min         3.014
_diffrn_source                   'Sealed Tube'
_exptl_absorpt_coefficient_mu    10.284
_exptl_absorpt_correction_T_max  0.627
_exptl_absorpt_correction_T_min  0.327
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private Communication'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    2.196
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             406
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.983
_refine_diff_density_min         -0.607
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     169
_refine_ls_number_reflns         2985
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0135
_refine_ls_R_factor_gt           0.0130
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0140P)^2^+1.3401P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0310
_refine_ls_wR_factor_ref         0.0312
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2936
_reflns_number_total             2985
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02809_si_002.cif
_cod_data_source_block           spider-14084
_cod_original_cell_volume        649.48(6)
_cod_database_code               4347153
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.233
_shelx_estimated_absorpt_t_max   0.627
_shelx_res_checksum              17708
_shelx_hkl_checksum              48605