β-Phosphorus hyperfine coupling constant in nitroxides: 5. Solvent effect
Audran, Gérard; Bosco, Lionel; Brémond, Paul; Butscher, Teddy; Franconi, Jean-Michel; Kabitaev, Kuanysh; Marque, Sylvain R. A.; Mellet, Philippe; Parzy, Elodie; Santelli, Maurice; Thiaudière, Eric; Viel, Stéphane; RSC Adv. 6 (2016) 5653–; doi:10.1039/C5RA23521A

data_7223890
_publ_section_title
;
 \b-Phosphorus hyperfine coupling constant in nitroxides: 5. Solvent
 effect
;
_journal_issue                   7
_journal_name_full               'RSC Adv.'
_journal_page_first              5653
_journal_paper_doi               10.1039/C5RA23521A
_journal_volume                  6
_journal_year                    2016
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C11 H23 N1 O5 P1'
_chemical_formula_sum            'C11 H23 N O5 P'
_chemical_formula_weight         280.27
_chemical_name_systematic
;
 ?
;
_chemical_properties_physical    Heat-sensitive
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2013-03-22T10:41:05-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2015-07-09 deposited with the CCDC.
2015-12-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 130.745(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3979(2)
_cell_length_b                   13.6246(3)
_cell_length_c                   13.7301(2)
_cell_measurement_reflns_used    14033
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.01
_cell_measurement_theta_min      2.46
_cell_measurement_wavelength     0.71073
_cell_volume                     1473.65(5)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'Omega + Phi scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.047
_diffrn_reflns_av_unetI/netI     0.0377
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14033
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         29.01
_diffrn_reflns_theta_min         2.46
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.199
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             604
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.485
_refine_diff_density_min         -0.37
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         3739
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0519
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0957P)^2^+0.3081P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1431
_refine_ls_wR_factor_ref         0.1718
_reflns_number_gt                2742
_reflns_number_total             3739
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c5ra23521a2.cif
_cod_data_source_block           lbtrans
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C11 H23 N1 O5 P1'
_cod_database_code               7223890