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_4105668
_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         'C28 H40 N P Rh, B F4'
_chemical_formula_sum            'C28 H40 B F4 N P Rh'
_chemical_formula_weight         611.30
_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
_audit_update_record
; 
2008-02-07   text and data added, srw 
;
_cell_angle_alpha                96.050(3)
_cell_angle_beta                 104.776(3)
_cell_angle_gamma                101.491(3)
_cell_formula_units_Z            2
_cell_length_a                   9.1929(5)
_cell_length_b                   9.2239(4)
_cell_length_c                   17.1717(9)
_cell_measurement_reflns_used    4390
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.30
_cell_measurement_theta_min      2.28
_cell_volume                     1360.82(12)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.0-1 (Bruker, 2004)'
_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)'
_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(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device       'Bruker Kappa/ApexII CCD'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  ga33yas
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_sigmaI/netI    0.0525
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16891
_diffrn_reflns_theta_full        25.85
_diffrn_reflns_theta_max         25.85
_diffrn_reflns_theta_min         2.28
_exptl_absorpt_coefficient_mu    0.732
_exptl_absorpt_correction_T_max  0.9629
_exptl_absorpt_correction_T_min  0.9301
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_description       prism
_exptl_crystal_F_000             632
_exptl_crystal_id                ga33yas
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (1 3 3) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.511
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         5095
_refine_ls_number_restraints     240
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0346
_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^)+(0.0314P)^2^+0.4437P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0684
_refine_ls_wR_factor_ref         0.0740
_reflns_number_gt                4167
_reflns_number_total             5095
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1057949_si_002.cif
_cod_data_source_block           ga33yas
_cod_original_sg_symbol_Hall     '-P 1 '
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4105668