Rhodium Phosphine-π-Arene Intermediates in the Hydroamination of Alkenes
Zhijian Liu; Hideaki Yamamichi; Sherzod T. Madrahimov; John F. Hartwig; Journal of the American Chemical Society 133 (2011) 2772–2782; doi:10.1021/ja1057949

data_4105672
_publ_section_title
;
 Rhodium Phosphine-\p-Arene Intermediates in the Hydroamination of Alkenes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2772
_journal_page_last               2782
_journal_paper_doi               10.1021/ja1057949
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C52 H72 Cl2 N2 P2 Rh2 '
_chemical_formula_sum            'C52 H72 Cl2 N2 P2 Rh2'
_chemical_formula_weight         1063.78
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
; 
? 
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.243(3)
_cell_length_b                   16.582(4)
_cell_length_c                   19.241(4)
_cell_measurement_reflns_used    963
_cell_measurement_temperature    193
_cell_measurement_theta_max      23.30
_cell_measurement_theta_min      2.46
_cell_volume                     4863.3(18)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'SMART V5.625 (Bruker, 2001)'
_computing_data_reduction
; 
SAINT V7.23A, XPREP V2005/2, SADABS V2007/4, TWINABS V2007/5 
(Bruker, 2005 & 2007) 
;
_computing_molecular_graphics
; 
SHELXTL V6.12 (Bruker, 2005), CrystalMaker v2.1.3 (CrystalMaker, 1994) 
;
_computing_publication_material  'XCIF V6.12 (Bruker, 2005)'
_computing_structure_refinement  'SHELXTL V6.12 (Bruker, 2005)'
_computing_structure_solution    'SHELXTL V6.12 (Bruker, 2005)'
_diffrn_ambient_temperature      193
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'Siemens Platform/CCD'
_diffrn_measurement_method       'profile data from \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  f22feas
_diffrn_reflns_av_R_equivalents  0.0662
_diffrn_reflns_av_sigmaI/netI    0.0344
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            50705
_diffrn_reflns_theta_full        25.39
_diffrn_reflns_theta_max         25.39
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    0.891
_exptl_absorpt_correction_T_max  0.9095
_exptl_absorpt_correction_T_min  0.8195
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS-2007/4 (Bruker, 2005)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_description       column
_exptl_crystal_F_000             2208
_exptl_crystal_id                f22feas
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (110) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.120
_refine_diff_density_max         1.172
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         4475
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_gt           0.0357
_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^)+(0.0549P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0824
_refine_ls_wR_factor_ref         0.0911
_reflns_number_gt                3107
_reflns_number_total             4475
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1057949_si_006.cif
_cod_data_source_block           f22feas
_cod_original_cell_volume        4863.5(19)
_cod_database_code               4105672