A novel scandium ortho-methoxynitrosobenzene-dimer complex: mechanistic implications for the nitroso-Diels???Alder reaction
Lightfoot, Andrew P.; Pritchard, Robin G.; Wan, Hayley; Warren, John E.; Whiting, Andrew; Chemical Communications  (2002) 2072–; doi:10.1039/b206366b

data_7111243
_publ_section_title
;
 A novel scandium ortho-methoxynitrosobenzene-dimer complex: mechanistic
 implications for the nitroso-Diels???Alder reaction
;
_journal_issue                   18
_journal_name_full               'Chemical Communications'
_journal_page_first              2072
_journal_paper_doi               10.1039/b206366b
_journal_year                    2002
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C21 H28 F9 N2 O16 S3 Sc1'
_chemical_formula_sum            'C21 H28 F9 N2 O16 S3 Sc'
_chemical_formula_weight         876.59
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_cell_angle_alpha                89.3120(10)
_cell_angle_beta                 80.7060(10)
_cell_angle_gamma                83.18
_cell_formula_units_Z            2
_cell_length_a                   11.04780
_cell_length_b                   11.35400
_cell_length_c                   14.70440
_cell_measurement_reflns_used    23643
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_measurement_wavelength     0.71073
_cell_volume                     1807.330(5)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.908
_diffrn_measured_fraction_theta_max 0.908
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.773886E-1
_diffrn_orient_matrix_UB_12      -0.176726E-1
_diffrn_orient_matrix_UB_13      0.272625E-1
_diffrn_orient_matrix_UB_21      0.49249E-1
_diffrn_orient_matrix_UB_22      -0.108951E-1
_diffrn_orient_matrix_UB_23      -0.632633E-1
_diffrn_orient_matrix_UB_31      0.108402E-1
_diffrn_orient_matrix_UB_32      0.862402E-1
_diffrn_orient_matrix_UB_33      -0.18877E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            30643
_diffrn_reflns_reduction_process
;
Scaled and merged with SORTAV
R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         4.6
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.491
_exptl_absorpt_correction_T_max  0.9082
_exptl_absorpt_correction_T_min  0.8667
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
?
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             892
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.4
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     581
_refine_ls_number_reflns         7524
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0294
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0265P)^2^+0.7760P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0714
_refine_ls_wR_factor_ref         0.0721
_reflns_number_gt                7324
_reflns_number_total             7524
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b206366bsup1.cif
_cod_data_source_block           2
_cod_original_cell_volume        1807.35(3)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7111243