Tetraorganylammonium Superoxide Compounds: Close to Unperturbed Superoxide Ions in the Solid State
Pascal D. C. Dietzel; Reinhard K. Kremer; Martin Jansen; Journal of the American Chemical Society 126 (2004) 4689–4696; doi:10.1021/ja039880i

data_4112420
_publ_contact_author_address
;Max-Planck-Institut f\"ur Festk\"orperforschung
 Heisenbergstr. 1 
 D-70569 Stuttgart
 Germany
;
_publ_contact_author_email       martin@jansen.mpi-stuttgart.mpg.de
_publ_contact_author_fax         +49-711-6891502
_publ_contact_author_name        'Martin Jansen'
_publ_contact_author_phone       +49-711-6891501
_publ_section_title
;
 Tetraorganylammonium Superoxide Compounds: Close to Unperturbed
 Superoxide Ions in the Solid State
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4689
_journal_page_last               4696
_journal_paper_doi               10.1021/ja039880i
_journal_volume                  126
_journal_year                    2004
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C9 H14 N 1+, O2 1-'
_chemical_formula_structural     '(N (C6 H5) (C H3)3) O2'
_chemical_formula_sum            'C9 H14 N O2'
_chemical_formula_weight         168.21
_chemical_name_systematic        'Trimethylphenylammonium hyperoxide'
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             99-10-11
_audit_creation_method           'STADI4, X-RED and SHELX-97'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.0496(11)
_cell_length_b                   9.9887(14)
_cell_length_c                   12.550(2)
_cell_measurement_reflns_used    36
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      17.2
_cell_measurement_theta_min      11.2
_cell_volume                     883.7(2)
_computing_cell_refinement       'STADI4 (STOE, 1996)'
_computing_data_collection       'STADI4 (STOE, 1996)'
_computing_data_reduction        'X-RED  (STOE, 1996)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(1)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'STOE STADI4 4-circle-diffractometer'
_diffrn_measurement_method
; Scan width (omega) = 1.20 - 1.40, scan ratio 2theta:omega = 1.00
  I(Net) and sigma(I) calculated according to Blessing (1987)
;
_diffrn_radiation_collimation    '0.8 mm'
_diffrn_radiation_detector       'NaI(Tl) scintillation counter'
_diffrn_radiation_monochromator  'planar graphite'
_diffrn_radiation_polarisn_norm  90
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_sigmaI/netI    0.0663
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            3022
_diffrn_reflns_theta_full        29.97
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         1.62
_diffrn_standards_decay_%        19.2
_diffrn_standards_interval_time  180
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_description       cuboid
_exptl_crystal_F_000             364
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.248
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         1492
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0439
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0666P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1057
_refine_ls_wR_factor_ref         0.1178
_reflns_d_resolution_high        0.711
_reflns_d_resolution_low         12.537
_reflns_limit_h_max              9
_reflns_limit_h_min              0
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                1210
_reflns_number_total             1492
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja039880isi20031201_083023.cif
_cod_data_source_block           NMe3PhO2
_cod_original_cell_volume        883.8(2)
_cod_database_code               4112420