Catalyst Design of Vaska-Type Iridium Complexes for Highly Efficient Synthesis of π-Conjugated Enamines
Tahara, Atsushi; Miyamoto, Yasumitsu; Aoto, Ryuta; Shigeta, Keisuke; Une, Yuta; Sunada, Yusuke; Motoyama, Yukihiro; Nagashima, Hideo; Organometallics 34 (2015) 4895–; doi:10.1021/acs.organomet.5b00636

data_4087840
_publ_section_title
;
 Catalyst Design of Vaska-Type Iridium Complexes for Highly Efficient
 Synthesis of \p-Conjugated Enamines
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              4895
_journal_paper_doi               10.1021/acs.organomet.5b00636
_journal_volume                  34
_journal_year                    2015
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C25 H24 Cl Ir N6 O P2'
_chemical_formula_sum            'C25 H24 Cl Ir N6 O P2'
_chemical_formula_weight         714.12
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 110.8047(11)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   10.1912(7)
_cell_length_b                   23.0093(15)
_cell_length_c                   12.0000(8)
_cell_measurement_reflns_used    12956
_cell_measurement_temperature    113
_cell_measurement_theta_max      30.69
_cell_measurement_theta_min      2.54
_cell_volume                     2630.4(3)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.1'
_computing_publication_material  'CrystalStructure 4.1 (Rigaku, 2014)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'Il Milione (Burla, et al., 2007)'
_diffrn_ambient_temperature      113
_diffrn_detector_area_resol_mean 28.445
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_Laue_measured_fraction_full 0.000
_diffrn_reflns_Laue_measured_fraction_max 0.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            16945
_diffrn_reflns_point_group_measured_fraction_full 0.000
_diffrn_reflns_point_group_measured_fraction_max 0.000
_diffrn_reflns_theta_full        27.490
_diffrn_reflns_theta_max         27.490
_diffrn_reflns_theta_min         3.218
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.344
_exptl_absorpt_correction_T_max  0.586
_exptl_absorpt_correction_T_min  0.495
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.803
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1392.00
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.98
_refine_diff_density_min         -6.49
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  4616 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.136(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.359
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     649
_refine_ls_number_reflns         10704
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0554
_refine_ls_shift/su_max          0.011
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0859P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1344
_refine_ls_wR_factor_ref         0.1350
_reflns_number_gt                10556
_reflns_number_total             10704
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om5b00636_si_002.cif
_cod_data_source_block           nat0051-Ir(Ppyrrolyl3)2(CO
_cod_database_code               4087840