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_7053437
_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_absolute_configuration unk
_chemical_formula_moiety         'C16 H15 N3'
_chemical_formula_sum            'C16 H15 N3'
_chemical_formula_weight         249.31
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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            4
_cell_length_a                   10.983(2)
_cell_length_b                   10.056(2)
_cell_length_c                   12.375(3)
_cell_measurement_reflns_used    5376
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.605
_cell_measurement_theta_min      2.61
_cell_volume                     1366.8(5)
_computing_cell_refinement       'Bruker-AXS APEX 2 Software'
_computing_data_collection       'Bruker-AXS APEX 2 Software'
_computing_data_reduction        'Bruker-AXS APEX 2 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      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'Bruker-AXS KAPPA APEX II 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  0.0317
_diffrn_reflns_av_sigmaI/netI    0.0169
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19525
_diffrn_reflns_theta_full        29.31
_diffrn_reflns_theta_max         29.31
_diffrn_reflns_theta_min         2.61
_exptl_absorpt_coefficient_mu    0.074
_exptl_absorpt_correction_T_max  0.9897
_exptl_absorpt_correction_T_min  0.9612
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.141
_refine_diff_density_min         -0.132
_refine_diff_density_rms         0.025
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         1953
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0351
_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^)+(0.0534P)^2^+0.0796P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0911
_refine_ls_wR_factor_ref         0.1032
_reflns_number_gt                1532
_reflns_number_total             1953
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b9nj00785g.txt
_cod_data_source_block           sb055
_cod_original_cell_volume        1366.7(5)
_cod_database_code               7053437