Functionalization of α-hydroxyphosphonates as a convenient route to N-tosyl-α-aminophosphonates
Cytlak, Tomasz; Skibińska, Monika; Kaczmarek, Patrycja; Kaźmierczak, Marcin; Rapp, Magdalena; Kubicki, Maciej; Koroniak, Henryk; RSC Advances 8 (2018) 11957–; doi:10.1039/C8RA01656A

data_7230388
_publ_section_title
;
 Functionalization of \a-hydroxyphosphonates as a convenient route to
 N-tosyl-\a-aminophosphonates
;
_journal_issue                   22
_journal_name_full               'RSC Advances'
_journal_page_first              11957
_journal_paper_doi               10.1039/C8RA01656A
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety         'C16 H21 F3 N O6 P'
_chemical_formula_sum            'C16 H21 F3 N O6 P'
_chemical_formula_weight         411.31
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-08-11 deposited with the CCDC.
2018-03-14 downloaded from the CCDC.
;
_cell_angle_alpha                108.225(10)
_cell_angle_beta                 112.480(12)
_cell_angle_gamma                90.483(10)
_cell_formula_units_Z            2
_cell_length_a                   10.1589(16)
_cell_length_b                   10.3309(11)
_cell_length_c                   10.8732(11)
_cell_measurement_reflns_used    1078
_cell_measurement_temperature    130(1)
_cell_measurement_theta_max      24.0030
_cell_measurement_theta_min      3.4980
_cell_volume                     990.8(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Mercury (MacRae et al., 2009)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      130(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2413
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '/w scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_av_unetI/netI     0.1084
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6885
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.992
_diffrn_reflns_theta_max         24.992
_diffrn_reflns_theta_min         3.643
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.197
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91606
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_description       plate
_exptl_crystal_F_000             428
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.713
_refine_diff_density_min         -0.351
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         3461
_refine_ls_number_restraints     140
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.2218
_refine_ls_R_factor_gt           0.1181
_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^)+(0.1893P)^2^+0.2757P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3060
_refine_ls_wR_factor_ref         0.3662
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1499
_reflns_number_total             3461
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ra01656a2.cif
_cod_data_source_block           38
_cod_database_code               7230388
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              61854