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_4083268
_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         'C26 H33 Cl Ir N4, C24 H20 B'
_chemical_formula_sum            'C50 H53 B Cl Ir N4'
_chemical_formula_weight         948.42
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           41
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'A 2 -2ab'
_symmetry_space_group_name_H-M   'A b a 2'
_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            8
_cell_length_a                   19.6897(2)
_cell_length_b                   25.1941(3)
_cell_length_c                   17.6879(2)
_cell_measurement_reflns_used    117757
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.631
_cell_measurement_theta_min      2.546
_cell_volume                     8774.34(17)
_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  0.0489
_diffrn_reflns_av_sigmaI/netI    0.0305
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            105270
_diffrn_reflns_theta_full        35.00
_diffrn_reflns_theta_max         35.00
_diffrn_reflns_theta_min         2.63
_exptl_absorpt_coefficient_mu    3.143
_exptl_absorpt_correction_T_max  0.587
_exptl_absorpt_correction_T_min  0.399
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SORTAV
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       piece
_exptl_crystal_F_000             3840
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.061
_refine_diff_density_min         -2.241
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.014(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         19269
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0237
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0244P)^2^+3.9436P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0498
_refine_ls_wR_factor_ref         0.0522
_reflns_number_gt                16610
_reflns_number_total             19269
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300550k_si_001.cif
_cod_data_source_block           compound_15a
_cod_original_sg_symbol_Hall     A2-2ac
_cod_original_sg_symbol_H-M      Aba2
_cod_database_code               4083268