Detangling Catalyst Modification Reactions from the Oxygen Evolution Reaction by Online Mass Spectrometry
Abril, Paula; del R\?ío, M. Pilar; Tejel, Cristina; Verhoeven, Tiny W. G. M.; Niemantsverdriet, J. W. Hans; Van der Ham, Cornelis J. M.; Kottrup, Konstantin G.; Hetterscheid, Dennis G. H.; ACS Catalysis  (2016) 7872–; doi:10.1021/acscatal.6b02800

data_4513978
_publ_section_title
;
 Detangling Catalyst Modification Reactions from the Oxygen Evolution
 Reaction by Online Mass Spectrometry
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              7872
_journal_paper_doi               10.1021/acscatal.6b02800
_journal_year                    2016
_chemical_formula_moiety         'C7H8Cl3IrNO3-, C7H8NO2+'
_chemical_formula_sum            'C14 H16 Cl3 Ir N2 O5'
_chemical_formula_weight         590.84
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                109.018(3)
_cell_angle_beta                 100.334(3)
_cell_angle_gamma                109.417(3)
_cell_formula_units_Z            2
_cell_length_a                   9.1361(19)
_cell_length_b                   10.454(2)
_cell_length_c                   10.987(2)
_cell_measurement_reflns_used    2499
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.294
_cell_measurement_theta_min      2.498
_cell_volume                     885.6(3)
_computing_cell_refinement       'SAINT+ v. 7.66A (Bruker AXS)'
_computing_data_collection       'APEX2 v. 4.0 (Bruker AXS, 2008)'
_computing_data_reduction        'SAINT+ v. 7.66A (Bruker AXS)'
_computing_molecular_graphics
;
ORTEP3 for Windows - L. J. Farrugia, 
J. Appl. Crystallogr. 1997, 30, 565.
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.895
_diffrn_measurement_device_type  'Bruker SMART APEX-II CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_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  0.0425
_diffrn_reflns_av_unetI/netI     0.0680
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.895
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9221
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.895
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.992
_diffrn_reflns_theta_min         2.071
_exptl_absorpt_coefficient_mu    8.018
_exptl_absorpt_correction_T_max  0.5601
_exptl_absorpt_correction_T_min  0.3929
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
  SADABS-2008/1: Area-Detector Absorption Correction. Bruker-AXS 
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.216
_exptl_crystal_description       plate
_exptl_crystal_F_000             564
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.447
_refine_diff_density_min         -1.462
_refine_diff_density_rms         0.231
_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     229
_refine_ls_number_reflns         4206
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0371
_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^)+(0.0283P)^2^+1.0341P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0693
_refine_ls_wR_factor_ref         0.0750
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3420
_reflns_number_total             4206
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs6b02800_si_002.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        885.7(3)
_cod_database_code               4513978
_shelx_estimated_absorpt_t_min   0.379
_shelx_estimated_absorpt_t_max   0.795
_shelxl_version_number           2013-4
_shelx_res_checksum              24877
_shelx_hkl_checksum              62743