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_7204401
_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_formula_moiety
;
2(C9 H12), (N O)^+^, (Cl6 Sb)^-^
;
_chemical_formula_sum            'C18 H24 Cl6 N O Sb'
_chemical_formula_weight         604.83
_chemical_name_systematic
; 
Mesitylene/nitrozonium hexachloroantimonate molecular complex 2:1 
;
_space_group_IT_number           8
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2y'
_symmetry_space_group_name_H-M   'C 1 m 1'
_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                 109.46(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.502(3)
_cell_length_b                   10.516(2)
_cell_length_c                   9.852(2)
_cell_measurement_reflns_used    3169
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      34.1
_cell_measurement_theta_min      2.6
_cell_volume                     1221.3(6)
_computing_cell_refinement       'SAINT V6.02 (Siemens, 1997-01)'
_computing_data_collection       'SMART V5.625 (Siemens, 1997-01)'
_computing_data_reduction        'SAINT & SADABS (Sheldrick, 2001)'
_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  0.0336
_diffrn_reflns_av_sigmaI/netI    0.0431
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8122
_diffrn_reflns_theta_max         35.68
_diffrn_reflns_theta_min         2.19
_diffrn_standards_decay_%        0.3
_diffrn_standards_number         284
_exptl_absorpt_coefficient_mu    1.795
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.781
_exptl_absorpt_correction_type   'Empirical (SADABS procedure)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.645
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.415
_refine_diff_density_min         -0.568
_refine_diff_density_rms         0.107
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.940
_refine_ls_goodness_of_fit_obs   0.980
_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     179
_refine_ls_number_reflns         4166
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.945
_refine_ls_restrained_S_obs      0.980
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_obs          0.0310
_refine_ls_shift/esd_max         -0.047
_refine_ls_shift/esd_mean        0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0349P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0658
_refine_ls_wR_factor_obs         0.0629
_reflns_number_observed          3559
_reflns_number_total             4169
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b202323g.txt
_cod_data_source_block           ros-csx
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0349P)^2^+0.0000P] 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^)+(0.0349P)^2^+0.0000P] 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        1221.2(4)
_cod_original_sg_symbol_H-M      Cm
_cod_database_code               7204401