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_4121001
_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_sum            'C23 H44 N O2 P2 Rh'
_chemical_formula_weight         531.44
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                100.065(2)
_cell_angle_beta                 96.798(2)
_cell_angle_gamma                105.223(2)
_cell_formula_units_Z            2
_cell_length_a                   8.3366(3)
_cell_length_b                   12.2975(4)
_cell_length_c                   13.5277(5)
_cell_measurement_reflns_used    5852
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.04
_cell_measurement_theta_min      3.37
_cell_volume                     1297.75(8)
_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 0.964
_diffrn_measured_fraction_theta_max 0.964
_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  0.0383
_diffrn_reflns_av_sigmaI/netI    0.0317
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17811
_diffrn_reflns_theta_full        66.58
_diffrn_reflns_theta_max         66.58
_diffrn_reflns_theta_min         3.37
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.617
_exptl_absorpt_correction_T_max  0.516
_exptl_absorpt_correction_T_min  0.426
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_description       block
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.500
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         4410
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0283
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0426P)^2^+0.4145P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0698
_refine_ls_wR_factor_ref         0.0716
_reflns_number_gt                3987
_reflns_number_total             4410
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4079539_si_002.cif
_cod_data_source_block           shelxl
_cod_database_code               4121001