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_4109008
_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            'C42 H57 Ir O P2'
_chemical_formula_weight         832.02
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
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_atom_sites_solution_hydrogens   geom
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_atom_sites_solution_secondary   difmap
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_cell_angle_beta                 114.286(1)
_cell_angle_gamma                90.00
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_cell_length_b                   39.671(3)
_cell_length_c                   9.3604(7)
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_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.42
_cell_measurement_theta_min      2.44
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_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 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0548
_diffrn_reflns_av_sigmaI/netI    0.0856
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_diffrn_reflns_limit_h_min       -16
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_diffrn_reflns_limit_k_min       -56
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
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_diffrn_reflns_theta_full        30.54
_diffrn_reflns_theta_max         30.54
_diffrn_reflns_theta_min         1.97
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.601
_exptl_absorpt_correction_T_max  0.9999
_exptl_absorpt_correction_T_min  0.7352
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   'Bruker SAINT (SADABS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_description       rod
_exptl_crystal_F_000             1696
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_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.909
_refine_diff_density_min         -2.245
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         11591
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_gt           0.0495
_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^)+(0.0328P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0853
_refine_ls_wR_factor_ref         0.0936
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_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0647194si20060716_051422.cif
_cod_data_source_block           ircovam
_cod_original_cell_volume        3829.1(5)
_cod_database_code               4109008