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_4112419
_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_formula_moiety         'C16 H36 N 1+, O2 1-, 2.5(N H3)'
_chemical_formula_sum            'C16 H43.5 N3.5 O2'
_chemical_formula_weight         317.04
_chemical_name_common
;
 Tetrabutylammonium superoxide ammoniate
;
_chemical_name_systematic
;
 Tetrabutylammonium hyperoxide ammoniate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 124.76(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   23.560(5)
_cell_length_b                   13.386(3)
_cell_length_c                   15.539(3)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      22.35
_cell_measurement_theta_min      4.3
_cell_volume                     4026(2)
_computing_cell_refinement       'Stoe IPDS software, Darmstadt 1998'
_computing_data_collection       'Stoe IPDS software, Darmstadt 1998'
_computing_data_reduction        'Stoe IPDS software, Darmstadt 1998'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       'phi oscillation'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56085
_diffrn_reflns_av_R_equivalents  0.0888
_diffrn_reflns_av_sigmaI/netI    0.0416
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            40651
_diffrn_reflns_theta_full        23.50
_diffrn_reflns_theta_max         23.50
_diffrn_reflns_theta_min         2.22
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.044
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.884
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, R.H., Acta Cryst. 1995, A51, 33'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.046
_exptl_crystal_description       'large block'
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.716
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         6001
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0786
_refine_ls_R_factor_gt           0.0576
_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^)+(0.0626P)^2^+3.5314P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1293
_refine_ls_wR_factor_ref         0.1413
_reflns_number_gt                4590
_reflns_number_total             6001
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja039880isi20031201_083001.cif
_cod_data_source_block           NBu4O2
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C16 H43.50 N3.50 O2'
_cod_database_code               4112419