Novel bis-arene (sandwich) complexes with NO+ acceptor. Isolation, X-ray crystallography and electronic structure
Rosokha, S. V.; Lindeman, S. V.; Kochi, J. K.; Journal of the Chemical Society, Perkin Transactions 2  (2002) 1468–; doi:10.1039/b202323g

data_7204399
_publ_section_title
;
 Novel bis-arene (sandwich) complexes with NO+ acceptor. Isolation,
 X-ray crystallography and electronic structure
;
_journal_issue                   8
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 2'
_journal_page_first              1468
_journal_paper_doi               10.1039/b202323g
_journal_year                    2002
_chemical_compound_source        'chemical synthesis'
_chemical_formula_moiety
;
2(C7 H8), (N O)^+^, (Cl6 Sb)^-^
;
_chemical_formula_sum            'C14 H16 Cl6 N O Sb'
_chemical_formula_weight         548.73
_chemical_name_systematic
; 
Toluene/nitrozonium hexachloroantimonate molecular complex 2:1 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.215(2)
_cell_length_b                   15.911(3)
_cell_length_c                   11.501(2)
_cell_measurement_reflns_used    4242
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      36.3
_cell_measurement_theta_min      2.2
_cell_volume                     2052.3(6)
_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  0.1157
_diffrn_reflns_av_sigmaI/netI    0.0900
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            25541
_diffrn_reflns_theta_max         36.31
_diffrn_reflns_theta_min         2.18
_diffrn_standards_decay_%        0.5
_diffrn_standards_number         131
_exptl_absorpt_coefficient_mu    2.127
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.803
_exptl_absorpt_correction_type   'Empirical (SADABS procedure)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.776
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.798
_refine_diff_density_min         -1.263
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.093
_refine_ls_goodness_of_fit_obs   1.168
_refine_ls_hydrogen_treatment
;
riding and rotating model with Uiso=1.2Uiso/eq of an adjacent carbon atom 
(1.5Uiso/eq for Me-hydrogens)
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     117
_refine_ls_number_reflns         4929
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.112
_refine_ls_restrained_S_obs      1.168
_refine_ls_R_factor_all          0.1657
_refine_ls_R_factor_obs          0.0610
_refine_ls_shift/esd_max         0.069
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0268P)^2^+4.1054P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1186
_refine_ls_wR_factor_obs         0.0828
_reflns_number_observed          2234
_reflns_number_total             4945
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b202323g.txt
_cod_data_source_block           raj-csx
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0268P)^2^+4.1054P] 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^)+(0.0268P)^2^+4.1054P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2052.3(7)
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               7204399