Dimerization of Alkynes Promoted by a Pincer-Ligated Iridium Complex. C-C Reductive Elimination Inhibited by Steric Crowding
Rajshekhar Ghosh; Xiawei Zhang; Patrick Achord; Thomas J. Emge; Karsten Krogh-Jespersen; Alan S. Goldman; Journal of the American Chemical Society 129 (2007) 853–866; doi:10.1021/ja0647194

data_4109004
_publ_contact_author_address
; 
 Department of Chemistry 
 Rutgers, The State University of New Jersey
 610 Taylor Road
 Piscataway, New Jersey  08854-8087  U.S.A. 
;
_publ_contact_author_email       agoldman@rutchem.rutgers.edu
_publ_contact_author_name        'Alan S. Goldman'
_publ_section_title
;
 Dimerization of Alkynes Promoted by a Pincer-Ligated Iridium Complex. C-C
 Reductive Elimination Inhibited by Steric Crowding
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              853
_journal_page_last               866
_journal_paper_doi               10.1021/ja0647194
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C41 H57 Ir P2'
_chemical_formula_weight         804.01
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
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_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_cell_angle_beta                 99.055(2)
_cell_angle_gamma                100.910(2)
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_cell_length_b                   10.7199(13)
_cell_length_c                   20.151(2)
_cell_measurement_reflns_used    6554
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      2.35
_cell_volume                     1824.3(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  '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  0.0805
_diffrn_reflns_av_sigmaI/netI    0.1240
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
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_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            17578
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         2.01
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.774
_exptl_absorpt_correction_T_max  0.9999
_exptl_absorpt_correction_T_min  0.6320
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SAINT (SADABS)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_description       plate
_exptl_crystal_F_000             820
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_exptl_crystal_size_min          0.02
_refine_diff_density_max         4.268
_refine_diff_density_min         -3.514
_refine_diff_density_rms         0.257
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         8025
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0951
_refine_ls_R_factor_gt           0.0677
_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^)+(0.0782P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1473
_refine_ls_wR_factor_ref         0.1568
_reflns_number_gt                6252
_reflns_number_total             8025
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0647194si20060716_051306.cif
_cod_data_source_block           ir39aly
_cod_original_cell_volume        1824.2(4)
_cod_database_code               4109004