Selective and clean synthesis of aminoalkyl-H-phosphinic acids from hypophosphorous acid by phospha-Mannich reaction
Urbanovský, Peter; Kotek, Jan; Císařová, Ivana; Hermann, Petr; RSC Advances 10 (2020) 21329–21349; doi:10.1039/D0RA03075A

data_7240648
_publ_section_title
;
 Selective and clean synthesis of aminoalkyl-H-phosphinic acids from
 hypophosphorous acid by phospha-Mannich reaction
;
_journal_issue                   36
_journal_name_full               'RSC Advances'
_journal_page_first              21329
_journal_page_last               21349
_journal_paper_doi               10.1039/D0RA03075A
_journal_volume                  10
_journal_year                    2020
_chemical_formula_moiety         'C9 H15 N O4 P2, H2 O'
_chemical_formula_sum            'C9 H17 N O5 P2'
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_atom_sites_solution_secondary   difmap
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_audit_update_record
;
2020-02-19 deposited with the CCDC.	2020-05-15 downloaded from the CCDC.
;
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'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
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_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150(2)
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_diffrn_radiation_monochromator  graphite
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_exptl_absorpt_coefficient_mu    0.350
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_exptl_crystal_description       plate
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_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.200
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_refine_diff_density_min         -0.274
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_refine_ls_abs_structure_details
;
 Flack x determined using 1096 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.04(4)
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
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_refine_ls_number_reflns         2908
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0308
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0435P)^2^+0.1163P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0734
_refine_ls_wR_factor_ref         0.0761
_reflns_Friedel_coverage         0.805
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.981
_reflns_number_gt                2630
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_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ra03075a3.cif
_cod_data_source_block           mpoll
_cod_depositor_comments
'Adding full bibliography for 7240636--7240653.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7240648
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.844
_shelx_estimated_absorpt_t_max   0.983
_shelx_res_checksum              72310