First α-deuterium nitroxides; synthesis and EPR study.
Toledo, Hila; Tumanskii, Boris; Sabirov, Denis Sh; Kaushansky, Alexander; Fridman, Natalia; Szpilman, Alex M.; Organic & biomolecular chemistry 17 (2019) 7900–7906; doi:10.1039/c9ob01127g

data_7157014
_publ_section_title
;
 First \a-deuterium nitroxides; synthesis and EPR study.
;
_journal_issue                   34
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              7900
_journal_page_last               7906
_journal_paper_doi               10.1039/c9ob01127g
_journal_volume                  17
_journal_year                    2019
_chemical_formula_moiety         'C48 H69 N O3 Si2 D2'
_chemical_formula_sum            'C48 H69 D2 N O3 Si2'
_chemical_formula_weight         766.23
_chemical_name_common            'Yoav333b (Hila)'
_chemical_properties_physical    Air-sensitive
_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   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-05-14 deposited with the CCDC.    2019-08-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.161(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.2809(13)
_cell_length_b                   16.3497(12)
_cell_length_c                   16.6811(13)
_cell_measurement_reflns_used    8117
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.081
_cell_measurement_theta_min      1.215
_cell_volume                     4569.8(6)
_computing_cell_refinement       'APEX2 v2010.7-0 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service v2010.7.0.0'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 95
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'APEX2 (Bruker AXS)'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0781
_diffrn_reflns_av_unetI/netI     0.0645
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            29270
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.081
_diffrn_reflns_theta_max         25.081
_diffrn_reflns_theta_min         1.215
_exptl_absorpt_coefficient_mu    0.117
_exptl_absorpt_correction_T_max  0.965
_exptl_absorpt_correction_T_min  0.958
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.114
_exptl_crystal_description       block
_exptl_crystal_F_000             1672
_exptl_crystal_recrystallization_method
'Solid after Flash Chromatography on silica gel and evaporation of solvent'
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.425
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     520
_refine_ls_number_reflns         8117
_refine_ls_number_restraints     154
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0789
_refine_ls_R_factor_gt           0.0506
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0770P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1347
_refine_ls_wR_factor_ref         0.1476
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5531
_reflns_number_total             8117
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ob01127g2.cif
_cod_data_source_block           yoav333b
_cod_depositor_comments          'Adding full bibliography for 7157014.cif.'
_cod_original_formula_sum        'C48 H69 N O3 Si2 D2'
_cod_database_code               7157014
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.973
_shelx_estimated_absorpt_t_max   0.983
_shelx_res_checksum              54161