Selective Dehydrogenative Coupling of Ethylene to Butadiene via an Iridacyclopentane Complex.
Gao, Yang; Emge, Thomas J.; Krogh-Jespersen, Karsten; Goldman, Alan S.; Journal of the American Chemical Society  (2018) –; doi:10.1021/jacs.7b11689

data_4127127
_publ_section_title
;
 Selective Dehydrogenative Coupling of Ethylene to Butadiene via an
 Iridacyclopentane Complex.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b11689
_journal_year                    2018
_chemical_formula_sum            'C23 H31 Ir N2 O3'
_chemical_formula_weight         575.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 108.945(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.6341(12)
_cell_length_b                   22.668(3)
_cell_length_c                   11.4074(16)
_cell_measurement_reflns_used    8383
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      31.00
_cell_measurement_theta_min      2.59
_cell_volume                     2111.7(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  SHELXL-2014/7
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            18032
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         1.797
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    6.350
_exptl_absorpt_correction_T_max  0.2664
_exptl_absorpt_correction_T_min  0.0843
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., 
 J. Appl. Cryst. 48 (2015) 3-10 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.811
_exptl_crystal_description       plate
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.030
_refine_diff_density_max         4.859
_refine_diff_density_min         -2.363
_refine_diff_density_rms         0.177
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.187
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4004
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      1.170
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0456
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0355P)^2^+21.6190P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1029
_refine_ls_wR_factor_ref         0.1049
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3698
_reflns_number_total             4004
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b11689_si_003.cif
_cod_data_source_block           irphebu1m_0m
_cod_database_code               4127127
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.143
_shelx_estimated_absorpt_t_max   0.832
_exptl_absorpt_special_details
; 
 Crystal faces: 
  
     H       K       L      d(mm) 
  
   1.000   0.000   0.000   0.25000 
  -1.000   0.000   0.000   0.25000 
   0.000   1.000   0.000   0.00500 
   0.000  -1.000   0.000   0.00500 
   0.000   0.000  -1.000   0.08500 
   0.000   0.000   1.000   0.08500 
  
   6 Faces  +   8 Corners  =  12 Edges  +  2 
  
 Cycle  1     Mu   0.000 mm-1     Rint  0.11504 
 Cycle  2     Mu   5.000 mm-1     Rint  0.10069 
 Cycle  3     Mu  13.090 mm-1     Rint  0.14364 
 Cycle  4     Mu   4.796 mm-1     Rint  0.10050 
 Cycle  5     Mu   4.307 mm-1     Rint  0.10034 
 Cycle  6     Mu   4.339 mm-1     Rint  0.10034 
 Cycle  7     Mu   4.323 mm-1     Rint  0.10034 
 Cycle  8     Mu   4.342 mm-1     Rint  0.10034 
 Cycle  9     Mu   4.394 mm-1     Rint  0.10034 
 All Rint values calculated using   20540 selected reflections only 
 Rint 0.1150 for mu = 0 and 0.1003 for mu =   4.359 mm-1 
 All Rint values calculated using   20540 selected reflections only 
 Minimum and maximum transmission coefficients = 0.39664 and 0.95730 
 Minimum and maximum t-bar = 0.0100 and 0.1896 mm 
;
_shelx_res_checksum              88568
_shelx_hkl_checksum              91912