Unexpected metal-mediated oxidation of hydroxymethyl groups to coordinated carboxylate groups by bis-cyclometalated iridium(iii) centers
Beyer, Beatrice; Ulbricht, Christoph; Winter, Andreas; Hager, Martin D.; Hoogenboom, Richard; Herzer, Nicole; Baumann, Stefan O.; Kickelbick, Guido; Görls, Helmar; Schubert, Ulrich S.; New Journal of Chemistry 34 (2010) 2622–; doi:10.1039/b9nj00785g

data_7053438
_publ_section_title
;
 Unexpected metal-mediated oxidation of hydroxymethyl groups to
 coordinated carboxylate groups by bis-cyclometalated iridium(iii) centers
;
_journal_issue                   11
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2622
_journal_paper_doi               10.1039/b9nj00785g
_journal_volume                  34
_journal_year                    2010
_chemical_formula_moiety         'C15 H13 N3 O'
_chemical_formula_sum            'C15 H13 N3 O'
_chemical_formula_weight         251.28
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   9.0879(4)
_cell_length_b                   9.1648(4)
_cell_length_c                   29.4080(14)
_cell_measurement_reflns_used    2752
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      56.428
_cell_measurement_theta_min      5.254
_cell_volume                     2449.36(19)
_computing_cell_refinement       'Bruker-AXS SAINT Software'
_computing_data_collection       'Bruker-AXS SMART Software'
_computing_data_reduction        'Bruker-AXS SAINT Software'
_computing_molecular_graphics    'Bruker-AXS SHELXTL Software'
_computing_publication_material  'Bruker-AXS SHELXTL Software'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      300(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'Bruker-AXS SMART CCD Detector'
_diffrn_measurement_method       omega-scans
_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  0.0204
_diffrn_reflns_av_sigmaI/netI    0.0137
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            19846
_diffrn_reflns_theta_full        28.33
_diffrn_reflns_theta_max         28.33
_diffrn_reflns_theta_min         2.63
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_T_max  0.9790
_exptl_absorpt_correction_T_min  0.9356
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.76
_exptl_crystal_size_mid          0.53
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.207
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         3038
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0461
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0798P)^2^+0.3381P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1254
_refine_ls_wR_factor_ref         0.1377
_reflns_number_gt                2452
_reflns_number_total             3038
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b9nj00785g.txt
_cod_data_source_block           use32
_cod_original_sg_symbol_Hall     '-P 2ac 2ab '
_cod_database_code               7053438