Electrophilic aromatic nitrosation. Isolation and X-ray crystallography of the metastable NO+ complex with nitrosoarene
Lindeman, Sergey V.; Bosch, Eric; Kochi, Jay K.; Journal of the Chemical Society, Perkin Transactions 2  (2000) 1919–; doi:10.1039/b002686g

data_7213346
_publ_section_title
;
 Electrophilic aromatic nitrosation. Isolation and X-ray crystallography
 of the metastable NO+ complex with nitrosoarene
;
_journal_issue                   9
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 2'
_journal_page_first              1919
_journal_paper_doi               10.1039/b002686g
_journal_year                    2000
_chemical_compound_source        'chemical synthesis'
_chemical_formula_moiety
;
(N O)^+^, (F6 P)^-^, (C7 H7 N O2), (C7 H8) 
;
_chemical_formula_sum            'C14 H15 F6 N2 O3 P'
_chemical_formula_weight         404.25
_chemical_name_systematic
; 
 Nitrozonium hexafluorophosphate/p-nitrosoanisol/toluene
 molecular complex 1:1:1 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                89.381(2)
_cell_angle_beta                 72.055(2)
_cell_angle_gamma                79.252(2)
_cell_formula_units_Z            2
_cell_length_a                   7.5078(6)
_cell_length_b                   10.7748(9)
_cell_length_c                   11.3584(9)
_cell_measurement_reflns_used    2009
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      32.0
_cell_measurement_theta_min      1.9
_cell_volume                     857.73(12)
_computing_cell_refinement       'SAINT V4.050 (Siemens, 1989-95)'
_computing_data_collection       'SMART V4.050 (Siemens, 1989-95)'
_computing_data_reduction        'SAINT & SADABS (Sheldrick, 1996)'
_computing_molecular_graphics    'XP V5.06 (Siemens, 1996)'
_computing_publication_material  'SHELXL-93 & XCIF V5.05 (Siemens, 1996)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measurement_device       'Siemens SMART'
_diffrn_measurement_method
;
\w-scan, frame range 0.3 deg, hemisphere
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_sigmaI/netI    0.0596
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7704
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.89
_diffrn_standards_decay_%        3.8
_diffrn_standards_number         95
_exptl_absorpt_coefficient_mu    0.239
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.879
_exptl_absorpt_correction_type   'Semi-empirical (SADABS procedure)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_density_method    none
_exptl_crystal_description       plate
_exptl_crystal_F_000             412
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.473
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.110
_refine_ls_goodness_of_fit_obs   1.205
_refine_ls_hydrogen_treatment
;
riding and rotating (for Me-hydrogens) model with Uiso=1.2Uiso/eq of
an adjacent atom (1.5Uiso/eq for Me-hydrogens)
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         3745
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.183
_refine_ls_restrained_S_obs      1.205
_refine_ls_R_factor_all          0.1354
_refine_ls_R_factor_obs          0.0772
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0403P)^2^+2.0700P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1728
_refine_ls_wR_factor_obs         0.1390
_reflns_number_observed          2613
_reflns_number_total             4084
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b002686gsup1.cif
_cod_data_source_block           eriklsx
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0403P)^2^+2.0700P] 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^)+(0.0403P)^2^+2.0700P] 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      P-1
_cod_database_code               7213346