Amino acid functionalisation using the 2-phosphaethynolate anion. A facile route to (phosphanyl)carbonyl-amino acids.
de Faria, Érica Neves; Jupp, Andrew; Goicoechea, Jose M.; Chem. Commun.  (2017) –; doi:10.1039/C7CC01285C

data_7120251
_publ_section_title
;
 Amino acid functionalisation using the 2-phosphaethynolate anion. A
 facile route to (phosphanyl)carbonyl-amino acids.
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC01285C
_journal_year                    2017
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C4 H7 N O3 P, C12 H24 K O6'
_chemical_formula_sum            'C16 H31 K N O9 P'
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_chemical_name_systematic
;
 [K(18-crown-6)][PH2C(O)NHCHCMeCOO]
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
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_symmetry_space_group_name_Hall  'P 2yb'
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_audit_update_record
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2017-02-16 deposited with the CCDC.
2017-06-08 downloaded from the CCDC.
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_cell_angle_alpha                90
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_computing_cell_refinement
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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,
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,
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    'WinGX (Farrugia, 2005)'
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_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0463
_diffrn_reflns_av_unetI/netI     0.0474
_diffrn_reflns_Laue_measured_fraction_full 0.999
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_diffrn_reflns_limit_h_max       10
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_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
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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.
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_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_description       needle
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.050
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_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.008(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
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_refine_ls_number_reflns         13248
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0421
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0724P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1104
_refine_ls_wR_factor_ref         0.1137
_reflns_Friedel_coverage         0.413
_reflns_Friedel_fraction_full    0.466
_reflns_Friedel_fraction_max     0.424
_reflns_number_gt                12013
_reflns_number_total             13248
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc01285c2.cif
_cod_data_source_block           shelx
_cod_database_code               7120251
_shelx_estimated_absorpt_t_min   0.301
_shelx_estimated_absorpt_t_max   0.858
_shelxl_version_number           2013-4
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