Transition Metal Migration upon Attempting the Wolff Rearrangement of an Ir(III) Five-Membered Metallacycle
Margarita Gómez; Margarita Paneque; Manuel L. Poveda; Eleuterio Alvarez; Journal of the American Chemical Society 129 (2007) 6092–6093; doi:10.1021/ja070360n

data_4109417
_publ_section_title
;
 Transition Metal Migration upon Attempting the Wolff Rearrangement of an
 Ir(III) Five-Membered Metallacycle
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6092
_journal_page_last               6093
_journal_paper_doi               10.1021/ja070360n
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         'C20 H26 B Ir N6 O3'
_chemical_formula_sum            'C20 H26 B Ir N6 O3'
_chemical_formula_weight         601.48
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m 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            4
_cell_length_a                   20.463(2)
_cell_length_b                   13.6577(16)
_cell_length_c                   7.9547(9)
_cell_measurement_reflns_used    3114
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.02
_cell_measurement_theta_min      2.75
_cell_volume                     2223.2(4)
_computing_cell_refinement       'SAINT+ v. 6.04 (Bruker-AXS, 2001)'
_computing_data_collection       'SMART v. 5.625 (Bruker-AXS, 2001)'
_computing_data_reduction        'SAINT+ v. 6.04 (Bruker-AXS, 2001)'
_computing_molecular_graphics    'xp program, SHELXTL v. 6.10, BRUKER, 2000'
_computing_publication_material  'XCIF program, SHELXTL v.6.10, Bruker 2000'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker-Nonius X8Apex II CCD area detector'
_diffrn_measurement_method       'phi and omega scans 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  0.0583
_diffrn_reflns_av_sigmaI/netI    0.0362
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            12462
_diffrn_reflns_theta_full        25.06
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         1.99
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    6.040
_exptl_absorpt_correction_T_max  0.5484
_exptl_absorpt_correction_T_min  0.2947
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS v. 2.03: Area-Detector Absorption Correction.
 (1997-2001) Bruker-AXS within SAINT+ package, v. 6.04
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.797
_exptl_crystal_description       needle
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.605
_refine_diff_density_min         -3.790
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         1997
_refine_ls_number_restraints     264
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0820
_refine_ls_R_factor_gt           0.0677
_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^)+(0.0485P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1224
_refine_ls_wR_factor_ref         0.1298
_reflns_number_gt                1639
_reflns_number_total             1997
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja070360nsi20070117_122221.cif
_cod_data_source_block           6
_cod_database_code               4109417