Nitrogen Atom Insertion into Ir-S and C-S Bonds Initiated by Photolysis of Iridium(III)-Azido-Dithiocarbamato Complexes
Takayoshi Suzuki; Antonio G. DiPasquale; James M. Mayer; Journal of the American Chemical Society 125 (2003) 10514–10515; doi:10.1021/ja0365779

data_4114117
_publ_contact_author
;
          Mayer, James M.
    Department of Chemistry
    University of Washington
    Seattle, WA 98195
    USA
;
_publ_contact_author_email       mayer@chem.washington.edu
_publ_section_title
;
 Nitrogen Atom Insertion into Ir-S and C-S Bonds Initiated by Photolysis
 of Iridium(III)-Azido-Dithiocarbamato Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10514
_journal_page_last               10515
_journal_paper_doi               10.1021/ja0365779
_journal_volume                  125
_journal_year                    2003
_chemical_formula_moiety         'C13 H21 Ir1 N4 S2'
_chemical_formula_sum            'C13 H21 Ir N4 S2'
_chemical_formula_weight         489.66
_chemical_name_common            suzuki03
_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                   15.5070(2)
_cell_length_b                   12.0280(3)
_cell_length_c                   8.8740(6)
_cell_measurement_reflns_used    243
_cell_measurement_temperature    130(2)
_cell_volume                     1655.16(12)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       KappaCCD
_computing_data_reduction        HKL-2000
_computing_molecular_graphics    'maXus, Zortep'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.883
_diffrn_measured_fraction_theta_max 0.883
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w 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  0.0397
_diffrn_reflns_av_sigmaI/netI    0.0645
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3363
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         3.49
_exptl_absorpt_coefficient_mu    8.315
_exptl_absorpt_correction_T_max  0.7885
_exptl_absorpt_correction_T_min  0.5560
_exptl_absorpt_correction_type   HKL-2000
_exptl_absorpt_process_details   'numerical, using redundancy'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.965
_exptl_crystal_description       prism
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.962
_refine_diff_density_min         -1.726
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    'H atoms riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     107
_refine_ls_number_reflns         1892
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0302
_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^)+(0.0125P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0536
_refine_ls_wR_factor_ref         0.0572
_reflns_number_gt                1451
_reflns_number_total             1892
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0365779si20030610_061224.cif
_cod_data_source_block           shelxl
_cod_original_formula_sum        'C13 H21 Ir1 N4 S2'
_cod_database_code               4114117