New chiral α-aminophosphine oxides and sulfides: an unprecedented rhodium-catalyzed ligand epimerization
Andrieu, Jacques; Camus, Jean-Michel; Poli, Rinaldo; Richard, Philippe; New Journal of Chemistry 25 (2001) 1015–; doi:10.1039/b100217l

data_7051103
_publ_section_title
;
 New chiral \a-aminophosphine oxides and sulfides: an unprecedented
 rhodium-catalyzed ligand epimerization
;
_journal_issue                   8
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1015
_journal_paper_doi               10.1039/b100217l
_journal_volume                  25
_journal_year                    2001
_chemical_formula_sum            'C54 H52 N2 P2 S2'
_chemical_formula_weight         855.04
_space_group_IT_number           4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2000-10-19T15:55:39-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 92.218(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.0532(4)
_cell_length_b                   18.5975(9)
_cell_length_c                   13.4262(8)
_cell_measurement_temperature    110(2)
_cell_volume                     2258.8(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.033
_diffrn_reflns_av_unetI/netI     0.0828
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14691
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         2.25
_exptl_absorpt_coefficient_mu    0.228
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             904
_refine_diff_density_max         0.271
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(5)
_refine_ls_extinction_coef       0.0028(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     549
_refine_ls_number_reflns         9440
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0425
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0311P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0753
_refine_ls_wR_factor_ref         0.0829
_reflns_number_gt                7329
_reflns_number_total             9440
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b100217l.txt
_cod_data_source_block           p31
_cod_database_code               7051103