Facile Generation and Isolation of π-Allyl Complexes from Aliphatic Alkenes and an Electron-Deficient Rh(III) Complex: Key Intermediates of Allylic C‒H Functionalization
Shibata, Yu; Kudo, Eiji; Sugiyama, Haruki; Uekusa, Hidehiro; Tanaka, Ken; Organometallics 35 (2016) 1547–; doi:10.1021/acs.organomet.6b00143

data_4088511
_publ_section_title
;
 Facile Generation and Isolation of \p-Allyl Complexes from Aliphatic
 Alkenes and an Electron-Deficient Rh(III) Complex: Key Intermediates of
 Allylic C--H Functionalization
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              1547
_journal_paper_doi               10.1021/acs.organomet.6b00143
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'Rh1, (C14 H19 O4), (C6 H11), Cl1'
_chemical_formula_sum            'C20 H30 Cl O4 Rh'
_chemical_formula_weight         472.80
_chemical_name_systematic        2
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 91.585(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1099(7)
_cell_length_b                   14.3425(9)
_cell_length_c                   15.8586(11)
_cell_measurement_reflns_used    15362
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      3.12
_cell_volume                     2071.3(3)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'PROCESS-AUTO (Rigaku, 1998)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 2008)'
_computing_publication_material  'SHELXL-2014/07 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'RIGAKU R-AXIS RAPID IP Area Detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0703
_diffrn_reflns_av_unetI/netI     0.0590
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19450
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.464
_diffrn_reflns_theta_min         3.118
_diffrn_source                   'rotating anode X-ray tube'
_exptl_absorpt_coefficient_mu    0.975
_exptl_absorpt_correction_T_max  0.895
_exptl_absorpt_correction_T_min  0.429
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Absorption was corrected by ABSCOR'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_description       plate
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.262
_exptl_crystal_size_mid          0.201
_exptl_crystal_size_min          0.117
_refine_diff_density_max         2.024
_refine_diff_density_min         -0.687
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         4685
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0543
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0650P)^2^+1.8807P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1261
_refine_ls_wR_factor_ref         0.1304
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3837
_reflns_number_total             4685
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00143_si_002.cif
_cod_data_source_block           shelxs
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4088511
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.784
_shelx_estimated_absorpt_t_max   0.895
_shelx_res_checksum              73739
_shelx_hkl_checksum              42364