Iridium(III) Cp* Complexes for the Efficient Hydroamination of Internal Alkynes
Gray, Katherine; Page, Michael J.; Wagler, Jörg; Messerle, Barbara A.; Organometallics 31 (2012) 6270–; doi:10.1021/om300550k

data_4083267
_publ_section_title
;
 Iridium(III) Cp* Complexes for the Efficient Hydroamination of Internal
 Alkynes
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              6270
_journal_paper_doi               10.1021/om300550k
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C27 H32 Cl Ir N2 P, C24 H20 B, 0.8(C6 H14)'
_chemical_formula_sum            'C55.8 H63.2 B Cl Ir N2 P'
_chemical_formula_weight         1031.31
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.5060(10)
_cell_angle_beta                 100.4750(10)
_cell_angle_gamma                92.0980(10)
_cell_formula_units_Z            2
_cell_length_a                   12.18970(10)
_cell_length_b                   12.96200(10)
_cell_length_c                   16.5879(2)
_cell_measurement_reflns_used    91131
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.142
_cell_measurement_theta_min      2.546
_cell_volume                     2550.27(4)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Nonius Collect, KappaCCD'
_computing_data_reduction
'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP32 for windows (Farugia)'
_computing_publication_material  'Ciftab (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius Kappa CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0510
_diffrn_reflns_av_sigmaI/netI    0.0367
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            87992
_diffrn_reflns_theta_full        33.00
_diffrn_reflns_theta_max         33.00
_diffrn_reflns_theta_min         2.63
_exptl_absorpt_coefficient_mu    2.738
_exptl_absorpt_correction_T_max  0.685
_exptl_absorpt_correction_T_min  0.472
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SORTAV
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       piece
_exptl_crystal_F_000             1052
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.701
_refine_diff_density_min         -1.854
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     573
_refine_ls_number_reflns         19221
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0286
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0401P)^2^+0.9469P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0726
_reflns_number_gt                17183
_reflns_number_total             19221
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300550k_si_001.cif
_cod_data_source_block           compound_14a
_cod_original_sg_symbol_Hall     -P1
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C55.80 H63.20 B Cl Ir N2 P'
_cod_database_code               4083267