Crystal and Electronic Structure of Stable Nitrenium Ions. A Comparison with Structurally Related Carbenes
Boche, Gernot; Andrews, Phil; Harms, Klaus; Marsch, Michael; Rangappa, Kanchugarakoppal S.; Schimeczek, Michael; Willeke, Christoph; Journal of the American Chemical Society 118 (1996) 4925–4930; doi:10.1021/ja9536274

data_1100464
_publ_contact_author
;
        Gernot Boche
        Fachbereich Chemie der Universit\"at
        Philipps Universit\"at Marburg
        Hans-Meerwein-Str.
        D-35032 Marburg
        Germany
;
_publ_contact_author_fax         '049 6421 288917 '
_publ_contact_author_phone       '049 6421 282030 '
_publ_section_title
;
 Crystal and Electronic Structure of Stable Nitrenium Ions. A Comparison
 with Structurally Related Carbenes
;
_journal_coden_ASTM              JACSAT
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4925
_journal_page_last               4930
_journal_paper_doi               10.1021/ja9536274
_journal_volume                  118
_journal_year                    1996
_chemical_formula_sum            'C10 H12 I N3'
_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     patterson
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 105.44(1)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.993(4)
_cell_length_b                   5.599(1)
_cell_length_c                   15.917(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      36.5
_cell_measurement_theta_min      21.1
_computing_cell_refinement       'CAD4 EXPRESS'
_computing_data_collection       'CAD4 EXPRESS'
_computing_data_reduction        'XCAD4 (Harms, 1993)'
_computing_molecular_graphics    SCHAKAL
_computing_publication_material  SHELXL
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measurement_device       'Enraf Nonius CAD4'
_diffrn_measurement_method       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  0.0099
_diffrn_reflns_av_sigmaI/netI    0.0201
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            2424
_diffrn_reflns_theta_min         2.66
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.729
_exptl_absorpt_correction_T_max  0.838
_exptl_absorpt_correction_T_min  0.621
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.714
_exptl_crystal_description       regular
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_ls_extinction_coef       0.00052(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.060
_refine_ls_goodness_of_fit_obs   1.075
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         2331
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0302
_refine_ls_R_factor_obs          0.0193
_refine_ls_shift/esd_max         0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0256P)^2^+2.0092P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0522
_refine_ls_wR_factor_obs         0.0485
_reflns_number_observed          1986
_reflns_number_total             2331
_reflns_observed_criterion       >2sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0256P)^2^+2.0092P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0256P)^2^+2.0092P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C10 H12 I1 N3'
_cod_database_code               1100464