4-Acetamido-3,3,5,5-[^2^H~4~]-2,2,6,6-tetra([^2^H~3~]methyl)piperidin-1-yloxyl 0.33-hydrate
Duskova, Jarmila; Jiri Labsky; Ivana Cisarova; Tereza Skalova; Jan Dohnalek; Jindrich Hasek; Acta Crystallographica Section C 62 (2006) o563–o566; doi:10.1107/S0108270106024814

data_2015577
_publ_section_title
;4-Acetamido-3,3,5,5-[^2^H~4~]-2,2,6,6-tetra([^2^H~3~]methyl)piperidin-1-yloxyl
 0.33-hydrate
;
_journal_coeditor_code           SK3034
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o563
_journal_page_last               o566
_journal_paper_doi               10.1107/S0108270106024814
_journal_volume                  62
_journal_year                    2006
_chemical_formula_moiety         'C11 H5 D16 N2 O2 , 0.33H2 O'
_chemical_formula_sum            'C11 H5.66 D16 N2 O2.33'
_chemical_formula_weight         235.34
_chemical_name_systematic
;4-Acetamido-3,3,5,5-[^2^H~4~]-2,2,6,6-tetra([^2^H~3~]methyl)piperidin-1-yloxyl
0.33-hydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                109.3510(10)
_cell_angle_beta                 101.6780(10)
_cell_angle_gamma                90.3250(10)
_cell_formula_units_Z            6
_cell_length_a                   10.6940(3)
_cell_length_b                   11.7120(3)
_cell_length_c                   16.0480(5)
_cell_measurement_reflns_used    36138
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     1851.41(9)
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_collection
'COLLECT (Nonius, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_data_reduction        'COLLECT and DENZO'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2005)'
_computing_publication_material  'SHELXL97 and DIAMOND'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.055
_diffrn_reflns_av_sigmaI/netI    0.0345
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            35956
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.89
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.079
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             722
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.289
_refine_diff_density_min         -0.276
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     663
_refine_ls_number_reflns         8420
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0481
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1025P)^2^+1.9749P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1288
_refine_ls_wR_factor_ref         0.1397
_reflns_number_gt                6918
_reflns_number_total             8420
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk3034.cif
_cod_data_source_block           I
_cod_database_code               2015577
_cod_database_fobs_code          2015577