Mild and high-yielding syntheses of diethyl phosphoramidate-stoppered [2]rotaxanes.
Hung, Wei-Chung; Liao, Kang-Shyang; Liu, Yi-Hung; Peng, Shie-Ming; Chiu, Sheng-Hsien; Organic letters 6 (2004) 4183–4186; doi:10.1021/ol0484557

data_1507001
_publ_section_title
;
 Mild and high-yielding syntheses of diethyl phosphoramidate-stoppered
 [2]rotaxanes.
;
_journal_issue                   23
_journal_name_full               'Organic letters'
_journal_page_first              4183
_journal_page_last               4186
_journal_paper_doi               10.1021/ol0484557
_journal_volume                  6
_journal_year                    2004
_chemical_formula_sum            'C50 H78 Cl3 F6 N3 O15.5 P3'
_chemical_formula_weight         1282.41
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.5430(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   56.1718(13)
_cell_length_b                   10.7872(2)
_cell_length_c                   22.9569(6)
_cell_measurement_temperature    295(2)
_cell_volume                     13629.1(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0687
_diffrn_reflns_av_sigmaI/netI    0.0751
_diffrn_reflns_limit_h_max       65
_diffrn_reflns_limit_h_min       -66
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            34129
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    0.279
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5384
_refine_diff_density_max         0.903
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.113
_refine_ls_extinction_coef       0.0019(4)
_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   1.224
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     756
_refine_ls_number_reflns         11975
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.224
_refine_ls_R_factor_all          0.2418
_refine_ls_R_factor_gt           0.1386
_refine_ls_shift/su_max          3.536
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3632
_refine_ls_wR_factor_ref         0.4067
_reflns_number_gt                5007
_reflns_number_total             11975
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol0484557si20040804_032747.cif
_cod_data_source_block           ic10734
_cod_original_formula_sum        'C50 H78 Cl3 F6 N3 O15.50 P3'
_cod_database_code               1507001