C-ON Bond Homolysis of Alkoxyamines, Part 11: Activation of the Nitroxyl Fragment.
Audran, Gérard; Brémond, Paul; Marque, Sylvain R. A.; Yamasaki, Toshihide; The Journal of organic chemistry 81 (2016) 1981–1988; doi:10.1021/acs.joc.5b02790

data_4036572
_publ_section_title
;
 C-ON Bond Homolysis of Alkoxyamines, Part 11: Activation of the Nitroxyl
 Fragment.
;
_journal_issue                   5
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              1981
_journal_page_last               1988
_journal_paper_doi               10.1021/acs.joc.5b02790
_journal_volume                  81
_journal_year                    2016
_chemical_formula_moiety         'C21 H38 N O5 P'
_chemical_formula_sum            'C21 H38 N O5 P'
_chemical_formula_weight         415.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-05-04
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Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
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_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3048
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_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.855
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  1 omega  -16.00   86.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       10.6548   38.0000   30.0000 102

  2 omega  -10.00   16.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.5611   57.0000  -30.0000 26

  3 omega   -7.00   32.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.5611  -99.0000 -150.0000 39

  4 omega  -18.00   52.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       10.6548  -99.0000 -150.0000 70

  5 omega  -68.00   44.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       10.6548  -77.0000   90.0000 112
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_diffrn_radiation_monochromator  mirror
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_diffrn_reflns_av_unetI/netI     0.0507
_diffrn_reflns_Laue_measured_fraction_full 0.998
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_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.897
_diffrn_reflns_theta_min         3.368
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.143
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90108
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
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_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.149
_exptl_crystal_description
;
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_exptl_crystal_F_000             904
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_exptl_crystal_size_min          0.14
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_refine_ls_structure_factor_coef Fsqd
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'w=1/[\s^2^(Fo^2^)+(0.0834P)^2^+1.3513P] where P=(Fo^2^+2Fc^2^)/3'
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_cod_database_code               4036572
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_reflns_odcompleteness_completeness 99.68
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_reflns_odcompleteness_theta     25.30
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2)
2.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C18(H18A,H18B), C20(H20A,H20B)
2.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5A), C6(H6), C7(H7), C8(H8)
2.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,
 H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C21(H21A,
 H21B,H21C)
2.e Idealised tetrahedral OH refined as rotating group:
 O5(H5)
;
_olex2_submission_special_instructions 'No special instructions were received'