Synthesis, physicochemical properties and antimicrobial activity of mono-/dinitroxyl amides.
Kavala, Miroslav; Brezová, Vlasta; Svorc, Lubomír; Vihonská, Zuzana; Olejníková, Petra; Moncol, Ján; Kožíšek, Jozef; Herich, Peter; Szolcsányi, Peter; Organic & biomolecular chemistry 12 (2014) 4491–4502; doi:10.1039/c4ob00302k

data_7153886
_publ_section_title
;
 Synthesis, physicochemical properties and antimicrobial activity of
 mono-/dinitroxyl amides.
;
_journal_issue                   25
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              4491
_journal_page_last               4502
_journal_paper_doi               10.1039/c4ob00302k
_journal_volume                  12
_journal_year                    2014
_chemical_formula_moiety         'C20 H34 F3 N3 O3, 0.5(C2 H6 O), 0.5(H2 O)'
_chemical_formula_sum            'C21 H38 F3 N3 O4'
_chemical_formula_weight         453.54
_chemical_name_systematic
;
N-(2,2,2-Trifluoroacetyl)-N,N-bis-
(1-oxo-2,2,6,6-tetramethylpiperidin-4-yl)-amine
1/2 ethanol hemihydrat
;
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 103.412(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2418(4)
_cell_length_b                   9.4098(2)
_cell_length_c                   19.4980(6)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.6460
_cell_measurement_theta_min      3.5860
_cell_volume                     2541.71(12)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2008)'
_computing_structure_solution    'OLEX2.SOLVE (Dolomanov et al., 2009)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.4353
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_unetI/netI     0.0162
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            30132
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.242
_diffrn_reflns_theta_min         2.941
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_T_max  0.971
_exptl_absorpt_correction_T_min  0.921
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_description       needle
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.750
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.210
_refine_diff_density_max         0.567
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         4546
_refine_ls_number_restraints     154
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0573
_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^)+(0.1161P)^2^+0.6399P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1690
_refine_ls_wR_factor_ref         0.1837
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3649
_reflns_number_total             4546
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4ob00302k2.cif
_cod_data_source_block           CCDC-953450
_cod_database_code               7153886
_shelx_estimated_absorpt_t_min   0.932
_shelx_estimated_absorpt_t_max   0.980
_shelxl_version_number           2013-4