Synthesis of Fluorinated β-Aminophosphonates and γ-Lactams
Concepción Alonso; María González; María Fuertes; Gloria Rubiales; Jose María Ezpeleta; Francisco Palacios; Journal of Organic Chemistry 78 (2013) 3858–3866; doi:10.1021/jo400281e

data_4028163
_publ_contact_author_address
;
Departamento de Quimica Organica I
Facultad de Farmacia
UPV/EHU
Paseo de la Universidad, 7
01006 Vitoria-Gasteiz
Spain
;
_publ_contact_author_email       francisco.palacios@ehu.es
_publ_contact_author_name        'Palacios, Francisco'
_publ_section_title
;
 Synthesis of Fluorinated \b-Aminophosphonates and \g-Lactams
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              3858
_journal_page_last               3866
_journal_paper_doi               10.1021/jo400281e
_journal_volume                  78
_journal_year                    2013
_chemical_formula_sum            'C18 H27 F3 N O5 P'
_chemical_formula_weight         425.38
_chemical_name_systematic
; 
Ethyl 3-diethoxyphosphinyl-5,5,5-trifluoro-4-
(4-tolylamino)pentanoate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
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_cell_angle_beta                 90.895(6)
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_cell_formula_units_Z            4
_cell_length_a                   11.6857(6)
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        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
        (compiled Jan 23 2012,18:06:46)
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        CrysAlisPro, Agilent Technologies,
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        (compiled Jan 23 2012,18:06:46)
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        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
        (compiled Jan 23 2012,18:06:46)
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_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
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_diffrn_ambient_temperature      100(2)
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_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_av_sigmaI/netI    0.0224
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
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_exptl_absorpt_coefficient_mu    1.613
_exptl_absorpt_correction_T_max  1.00000
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_description       prism
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.308
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
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_refine_ls_number_reflns         4041
_refine_ls_number_restraints     89
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_refine_ls_R_factor_all          0.0397
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_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0492P)^2^+1.1954P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0940
_refine_ls_wR_factor_ref         0.0965
_reflns_number_gt                3704
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_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo400281e_si_004.cif
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