The Effect of Structure on Nitroxide EPR Spectral Linewidth
Scott R. Burks; Mallory A. Makowsky; Zachary A. Yaffe; Chad Hoggle; Pei Tsai; Sukumaran Muralidharan; Michael K. Bowman; Joseph P.Y. Kao; Gerald M. Rosen; Journal of Organic Chemistry 75 (2010) 4737–4741; doi:10.1021/jo1005747

data_4025533
_publ_section_title
;
 The Effect of Structure on Nitroxide EPR Spectral Linewidth
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              4737
_journal_page_last               4741
_journal_paper_doi               10.1021/jo1005747
_journal_volume                  75
_journal_year                    2010
_chemical_formula_moiety         'C12 H20 N O3'
_chemical_formula_sum            'C12 H20 N O3'
_chemical_formula_weight         226.29
_chemical_name_common            nitroxide
_chemical_name_systematic
;
piperidine-1-oxyl-4-methylene acetic acid methyl ester
;
_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_creation_method           'SHELXL-97 & ZCIF'
_cell_angle_alpha                90.00
_cell_angle_beta                 109.5925(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.7657(7)
_cell_length_b                   15.5387(14)
_cell_length_c                   11.2639(10)
_cell_measurement_reflns_used    5154
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      25.5
_cell_measurement_theta_min      2.3
_cell_volume                     1280.5(2)
_computing_cell_refinement       Apex2
_computing_data_collection       'Apex2 (Bruker, 2005)'
_computing_data_reduction        Apex2
_computing_molecular_graphics    'XSHEL (Bruker, 2004)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      250(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 11.198
_diffrn_detector_type            'Bruker Smart Apex II'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      610,610,610
_diffrn_measurement_device_type  'three-circle diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'glass capillary'
_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      0.1280062
_diffrn_orient_matrix_UB_12      -0.0106648
_diffrn_orient_matrix_UB_13      0.0570333
_diffrn_orient_matrix_UB_21      -0.0466372
_diffrn_orient_matrix_UB_22      -0.0408026
_diffrn_orient_matrix_UB_23      0.0508362
_diffrn_orient_matrix_UB_31      0.0110672
_diffrn_orient_matrix_UB_32      -0.0486115
_diffrn_orient_matrix_UB_33      -0.0551647
_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  0.0220
_diffrn_reflns_av_sigmaI/netI    0.0216
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9232
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.32
_diffrn_source_current           30.00
_diffrn_source_voltage           50.00
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_T_max  0.967
_exptl_absorpt_correction_T_min  0.914
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.174
_exptl_crystal_description       bulk
_exptl_crystal_F_000             492
_exptl_crystal_id
'UMBC/Kao piperidine-1-oxyl-4-methylene acetic acid methyl ester'
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.439
_refine_diff_density_min         -0.157
_refine_diff_density_rms         0.034
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     161
_refine_ls_number_reflns         2268
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0488
_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^)+(0.005P)^2^+0.9535P], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0938
_refine_ls_wR_factor_ref         0.0970
_reflns_number_gt                1909
_reflns_number_total             2268
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo1005747_si_001.cif
_cod_data_source_block           1819
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4025533
_diffrn_measurement_frame_width-ccd -0.30
_diffrn_measurement_total_frames-ccd 1830
_diffrn_measurement_frame_time-ccd 45
_diffrn_measurement_total_time-ccd 25.9
_diffrn_detector_distance-ccd    5.800
_diffrn_measurement_frame_size-ccd 512