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_4109416
_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 O2'
_chemical_formula_sum            'C20 H26 B Ir N6 O2'
_chemical_formula_weight         585.48
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 94.738(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.0966(6)
_cell_length_b                   19.5568(13)
_cell_length_c                   14.0294(10)
_cell_measurement_reflns_used    6008
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.41
_cell_measurement_theta_min      2.54
_cell_volume                     2213.9(3)
_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 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0420
_diffrn_reflns_av_sigmaI/netI    0.0472
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20959
_diffrn_reflns_theta_full        29.66
_diffrn_reflns_theta_max         29.66
_diffrn_reflns_theta_min         1.79
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    6.059
_exptl_absorpt_correction_T_max  0.2691
_exptl_absorpt_correction_T_min  0.1140
_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    1.757
_exptl_crystal_description       block
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.965
_refine_diff_density_min         -0.738
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         6187
_refine_ls_number_restraints     296
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0679
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+150.6545P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1623
_refine_ls_wR_factor_ref         0.1645
_reflns_number_gt                5623
_reflns_number_total             6187
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja070360nsi20070117_122202.cif
_cod_data_source_block           5
_cod_database_code               4109416