A concise route to beta-Cyclopropyl amino acids utilizing 1,2-dioxines and stabilized phosphonate nucleophiles.
Avery, Thomas D.; Greatrex, Ben W.; Pedersen, Daniel Sejer; Taylor, Dennis K.; Tiekink, Edward R. T.; The Journal of organic chemistry 73 (2008) 2633–2640; doi:10.1021/jo7024256

data_4029547
_publ_section_title
;
 A concise route to beta-Cyclopropyl amino acids utilizing 1,2-dioxines
 and stabilized phosphonate nucleophiles.
;
_journal_issue                   7
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              2633
_journal_page_last               2640
_journal_paper_doi               10.1021/jo7024256
_journal_volume                  73
_journal_year                    2008
_chemical_formula_moiety         'C26 H41 N O7 Si'
_chemical_formula_sum            'C26 H41 N O7 Si'
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_symmetry_space_group_name_H-M   'P -1'
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_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
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_cell_angle_beta                 80.766(15)
_cell_angle_gamma                88.909(16)
_cell_formula_units_Z            2
_cell_length_a                   8.148(2)
_cell_length_b                   10.579(3)
_cell_length_c                   17.328(5)
_cell_measurement_reflns_used    2884
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.3
_cell_measurement_theta_min      2.5
_cell_volume                     1420.1(7)
_computing_cell_refinement       CrystalClear
_computing_data_collection
'CrystalClear (Rigaku Americas Corporation, 2005)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.848
_diffrn_measured_fraction_theta_max 0.848
_diffrn_measurement_device_type  AFC12\k/SATURN724
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
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_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
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_diffrn_reflns_limit_h_max       9
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_diffrn_reflns_limit_l_min       -20
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_diffrn_reflns_theta_full        25.6
_diffrn_reflns_theta_max         25.6
_diffrn_reflns_theta_min         2.5
_diffrn_standards_decay_%        '< 1'
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.124
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.764
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             548
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.31
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_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.17
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         4533
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.17
_refine_ls_R_factor_all          0.090
_refine_ls_R_factor_gt           0.071
_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^)+(0.0707P)^2^+0.3657P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.153
_refine_ls_wR_factor_ref         0.164
_reflns_number_gt                3670
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_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            jo7024256-file006.cif
_cod_data_source_block           28f
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