Rhodium(I) and Iridium(I) Complexes with Bidentate Phosphine−Pyrazolyl Ligands: Highly Efficient Catalysts for the Hydroamination Reaction
Field, Leslie D.; Messerle, Barbara A.; Vuong, Khuong Q.; Turner, Peter; Failes, Tim; Organometallics 26 (2007) 2058–; doi:10.1021/om070057v

data_4073084
_publ_section_title
;
 Rhodium(I) and Iridium(I) Complexes with Bidentate
 Phosphine&#x2212;Pyrazolyl Ligands:&#x00A0; Highly Efficient Catalysts
 for the Hydroamination Reaction
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              2058
_journal_paper_doi               10.1021/om070057v
_journal_volume                  26
_journal_year                    2007
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C20 H21 Cl Ir N2 O P, C H2 Cl2'
_chemical_formula_sum            'C21 H23 Cl3 Ir N2 O P'
_chemical_formula_weight         648.95
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                   11.2909(18)
_cell_length_b                   19.373(3)
_cell_length_c                   20.890(3)
_cell_measurement_reflns_used    1022
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.243
_cell_measurement_theta_min      4.031
_cell_volume                     4569.4(12)
_computing_cell_refinement       'SAINT (Bruker,1995)'
_computing_data_collection       'SMART (Bruker,1995)'
_computing_data_reduction        'SAINT and XPREP (Bruker 1995)'
_computing_molecular_graphics    'WinGX (Farrugia, 1999)'
_computing_publication_material  ORTEP3
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       \w
_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  0.0788
_diffrn_reflns_av_sigmaI/netI    0.0575
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            43853
_diffrn_reflns_theta_full        28.02
_diffrn_reflns_theta_max         28.02
_diffrn_reflns_theta_min         1.95
_diffrn_standards_decay_%        -0.08
_diffrn_standards_number         417
_exptl_absorpt_coefficient_mu    6.280
_exptl_absorpt_correction_T_max  0.5724
_exptl_absorpt_correction_T_min  0.1269
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'Gaussian (Coppens et al., 1965)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.887
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'flat needle'
_exptl_crystal_F_000             2512
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.625
_refine_diff_density_min         -2.053
_refine_diff_density_rms         0.186
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.000(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     528
_refine_ls_number_reflns         10728
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0439P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0814
_refine_ls_wR_factor_ref         0.0832
_reflns_number_gt                9465
_reflns_number_total             10728
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om070057vsi20070118_104046.cif
_cod_data_source_block           bam22
_cod_original_cell_volume        4569.3(13)
_cod_original_sg_symbol_H-M      P212121
_cod_original_formula_sum        'C21 H23 Cl3 Ir1 N2 O P'
_cod_database_code               4073084