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_4083271
_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         'C19 H27 Cl N4 Rh, C24 H20 B'
_chemical_formula_sum            'C43 H47 B Cl N4 Rh'
_chemical_formula_weight         769.02
_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                 95.7040(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.2866(5)
_cell_length_b                   14.6089(4)
_cell_length_c                   18.9761(6)
_cell_measurement_reflns_used    4901
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      25.39
_cell_measurement_theta_min      2.41
_cell_volume                     3665.1(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep32 (Farugia)'
_computing_publication_material  'Shelx-97/ciftab(Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'APEX2 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  0.0580
_diffrn_reflns_av_sigmaI/netI    0.0671
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            31321
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    0.576
_exptl_absorpt_correction_T_max  0.9773
_exptl_absorpt_correction_T_min  0.8962
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.729
_refine_diff_density_min         -0.614
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     521
_refine_ls_number_reflns         8843
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0762
_refine_ls_R_factor_gt           0.0415
_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^)+(0.0431P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0837
_refine_ls_wR_factor_ref         0.0910
_reflns_number_gt                6233
_reflns_number_total             8843
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300550k_si_001.cif
_cod_data_source_block           compound_16b
_cod_original_sg_symbol_Hall     -P2yn
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4083271