Hydroxylamine as an Oxygen Nucleophile. Structure and Reactivity of Ammonia Oxide
Anthony J. Kirby; John E. Davies; Tiago A. S. Brandão; Pedro F. da Silva; Willian R. Rocha; Faruk Nome; Journal of the American Chemical Society 128 (2006) 12374–12375; doi:10.1021/ja065147q

data_4110928
_publ_section_title
;
 Hydroxylamine as an Oxygen Nucleophile. Structure and Reactivity of
 Ammonia Oxide
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12374
_journal_page_last               12375
_journal_paper_doi               10.1021/ja065147q
_journal_volume                  128
_journal_year                    2006
_chemical_formula_moiety         'H4 N O, H3 N O, Cl'
_chemical_formula_sum            'Cl H7 N2 O2'
_chemical_formula_weight         102.53
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 92.3450(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.21670(10)
_cell_length_b                   8.1338(2)
_cell_length_c                   7.0381(2)
_cell_measurement_reflns_used    8047
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      45.29
_cell_measurement_theta_min      1.0
_cell_volume                     412.785(17)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius B.V. 1998)'
_computing_data_reduction
;

 HKL Denzo and Scalepack (Otwinowski & Minor 1997)

;
_computing_publication_material  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_solution    'SIR-92 (Altomare et al. 1994)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Thin slice \w and \f scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_sigmaI/netI    0.0263
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12868
_diffrn_reflns_theta_full        45.27
_diffrn_reflns_theta_max         45.27
_diffrn_reflns_theta_min         3.78
_exptl_absorpt_coefficient_mu    0.762
_exptl_absorpt_correction_T_max  0.951
_exptl_absorpt_correction_T_min  0.884
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;

multi-scan from symmetry-related measurements 

 Sortav (Blessing 1995)

;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.650
_exptl_crystal_description       plate
_exptl_crystal_F_000             216
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.388
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     53
_refine_ls_number_reflns         3441
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0227
_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^)+(0.0151P)^2^+0.0827P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0558
_refine_ls_wR_factor_ref         0.0576
_reflns_number_gt                3071
_reflns_number_total             3441
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja065147qsi20060728_044327.cif
_cod_data_source_block           x
_cod_original_sg_symbol_Hall     -P2ybc
_cod_database_code               4110928