Synthesis and stability of cyclic α-hydrogen nitroxides.
Toledo, Hila; Amar, Michal; Bar, Sukanta; Iron, Mark A.; Fridman, Natalia; Tumanskii, Boris; Shimon, Linda J. W.; Botoshansky, Mark; Szpilman, Alex M.; Organic & biomolecular chemistry 13 (2015) 10726–10733; doi:10.1039/c5ob01443c

data_7154666
_publ_section_title
;
 Synthesis and stability of cyclic \a-hydrogen nitroxides.
;
_journal_issue                   43
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              10726
_journal_page_last               10733
_journal_paper_doi               10.1039/c5ob01443c
_journal_volume                  13
_journal_year                    2015
_chemical_formula_moiety         '2(C48 H70 N O3 Si2), 0.5(C6 H14)'
_chemical_formula_sum            'C49.5 H73.5 N O3 Si2'
_chemical_formula_weight         786.77
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_block_doi                 10.5517/cc11qvtf
_audit_creation_method           SHELXL-97
_audit_update_record
;
2013-12-04 deposited with the CCDC.
2015-08-24 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 131.6830(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.8707(3)
_cell_length_b                   37.2414(7)
_cell_length_c                   21.2432(4)
_cell_measurement_reflns_used    80183
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.59
_cell_measurement_theta_min      2.09
_cell_volume                     9377.1(3)
_computing_cell_refinement       'Bruker Apex2'
_computing_data_collection       'Bruker Apex2'
_computing_data_reduction        'Bruker Apex2'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker KappaApexII CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0555
_diffrn_reflns_av_sigmaI/netI    0.0665
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            80183
_diffrn_reflns_theta_full        27.59
_diffrn_reflns_theta_max         27.59
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    0.115
_exptl_absorpt_correction_T_max  0.9908
_exptl_absorpt_correction_T_min  0.9829
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.115
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3436
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.071
_refine_diff_density_min         -0.720
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1103
_refine_ls_number_reflns         21575
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0998
_refine_ls_R_factor_gt           0.0619
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0819P)^2^+6.2093P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1528
_refine_ls_wR_factor_ref         0.1738
_reflns_number_gt                14626
_reflns_number_total             21575
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ob01443c2.cif
_cod_data_source_block           sa1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 7154666--7154672.cif.
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C49.50 H73.50 N O3 Si2'
_cod_database_code               7154666