Intramolecular Hydroamination of Unbiased and Functionalized Primary Aminoalkenes Catalyzed by a Rhodium Aminophosphine Complex
Lisa D. Julian; John F. Hartwig; Journal of the American Chemical Society 132 (2010) 13813–13822; doi:10.1021/ja1052126

data_4103142
_publ_contact_author
; 
Danielle L. Gray 
University of Illinois 
School of Chemical Sciences, Box 59-1 
505 South Mathews Avenue 
Urbana, Illinois  61801 
USA 
;
_publ_contact_author_email       dgray@illinois.edu
_publ_contact_author_fax         '1  217 244 8068'
_publ_contact_author_phone       '1  217 244 1708'
_publ_section_title
;
 Intramolecular Hydroamination of Unbiased and Functionalized Primary
 Aminoalkenes Catalyzed by a Rhodium Aminophosphine Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13813
_journal_page_last               13822
_journal_paper_doi               10.1021/ja1052126
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C33 H55 N5 O P2 Rh, B F4'
_chemical_formula_sum            'C33 H55 B F4 N5 O P2 Rh'
_chemical_formula_weight         789.48
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
; 
2008-12-17   text and data added, dlg 
;
_cell_angle_alpha                90.00
_cell_angle_beta                 104.227(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.3079(12)
_cell_length_b                   16.9887(11)
_cell_length_c                   24.5185(17)
_cell_measurement_reflns_used    2543
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      18.20
_cell_measurement_theta_min      2.40
_cell_volume                     7795.8(9)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  ba81da
_diffrn_reflns_av_R_equivalents  0.2497
_diffrn_reflns_av_sigmaI/netI    0.2289
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            80549
_diffrn_reflns_theta_full        20.81
_diffrn_reflns_theta_max         20.81
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    0.571
_exptl_absorpt_correction_T_max  0.9794
_exptl_absorpt_correction_T_min  0.9383
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tabular
_exptl_crystal_F_000             3296
_exptl_crystal_id                ba81da
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (3 2 -4) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.608
_refine_diff_density_min         -0.556
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1345
_refine_ls_number_reflns         8164
_refine_ls_number_restraints     2622
_refine_ls_restrained_S_all      0.846
_refine_ls_R_factor_all          0.2036
_refine_ls_R_factor_gt           0.0762
_refine_ls_shift/su_max          0.053
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1561P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1877
_refine_ls_wR_factor_ref         0.2532
_reflns_number_gt                3065
_reflns_number_total             8164
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1052126_si_002.cif
_cod_data_source_block           ba81da
_cod_original_sg_symbol_Hall     '-P 2ybc '
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_database_code               4103142