Stability and Dynamic Processes in 16VE Iridium(III) Ethyl Hydride and Rhodium(I) σ-Ethane Complexes: Experimental and Computational Studies
Marc D. Walter; Peter S. White; Cynthia K. Schauer; Maurice Brookhart; Journal of the American Chemical Society 135 (2013) 15933–15947; doi:10.1021/ja4079539

data_4121000
_publ_section_title
;
 Stability and Dynamic Processes in 16VE Iridium(III) Ethyl Hydride and
 Rhodium(I) \s-Ethane Complexes: Experimental and Computational Studies
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15933
_journal_page_last               15947
_journal_paper_doi               10.1021/ja4079539
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C24 H46 Ir N O2 P2'
_chemical_formula_sum            'C24 H46 Ir N O2 P2'
_chemical_formula_weight         634.76
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
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_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.280(2)
_cell_angle_beta                 104.437(2)
_cell_angle_gamma                101.715(2)
_cell_formula_units_Z            2
_cell_length_a                   8.4556(2)
_cell_length_b                   10.6550(2)
_cell_length_c                   16.3491(4)
_cell_measurement_reflns_used    7553
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.56
_cell_measurement_theta_min      2.84
_cell_volume                     1372.09(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_sigmaI/netI    0.0610
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12837
_diffrn_reflns_theta_full        69.94
_diffrn_reflns_theta_max         69.94
_diffrn_reflns_theta_min         2.84
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.659
_exptl_absorpt_correction_T_max  0.6178
_exptl_absorpt_correction_T_min  0.3611
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   SADABS-2008/1
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_description       plate
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.254
_refine_diff_density_min         -1.226
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         4882
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0424
_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^)+(0.0789P)^2^+0.1958P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1124
_refine_ls_wR_factor_ref         0.1150
_reflns_number_gt                4505
_reflns_number_total             4882
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4079539_si_001.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        1372.09(5)
_cod_database_code               4121000