C−S Bond Activation of Two Novel Asymmetric α-azo-Ketenedithioacetals Using Fe2(CO)9
Ortega-Alfaro, M. Carmen; Alcantara, Olga; Orrala, Manuel; López-Cortés, José G.; Toscano, Ruben A.; Alvarez-Toledano, Cecilio; Organometallics 26 (2007) 1895–; doi:10.1021/om060953r

data_4072697
_publ_section_title
;
 C&#x2212;S Bond Activation of Two Novel Asymmetric
 \a-azo-Ketenedithioacetals Using Fe2(CO)9
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              1895
_journal_paper_doi               10.1021/om060953r
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         'C10 H16 N2 O S2'
_chemical_formula_sum            'C10 H16 N2 O S2'
_chemical_formula_weight         244.37
_chemical_name_systematic
; 
1-tert-Butylazo-1-[1,3]dithiolan-2-ylidene-propan-2-one
;
_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-97
_cell_angle_alpha                84.710(10)
_cell_angle_beta                 84.730(10)
_cell_angle_gamma                80.610(10)
_cell_formula_units_Z            2
_cell_length_a                   5.832(3)
_cell_length_b                   5.833(3)
_cell_length_c                   19.326(4)
_cell_measurement_reflns_used    1456
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      32.43
_cell_measurement_theta_min      3.19
_cell_volume                     643.9(5)
_computing_cell_refinement       'SMART V 5.625'
_computing_data_collection       'SMART V 5.625'
_computing_data_reduction        'SAINT V 6.23C'
_computing_molecular_graphics    'SHELXTL V 6.10 (Sheldrick, 2000)'
_computing_publication_material  'SHELXTL V 6.10 (Sheldrick, 2000)'
_computing_structure_refinement  'SHELXTL V 6.10 (Sheldrick, 2000)'
_computing_structure_solution    'SIR97 (Altomare et al, 1999)'
_diffrn_ambient_temperature      294(2)
_diffrn_detector_area_resol_mean 0.661
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker Smart Apex CCD diffractometer'
_diffrn_measurement_method       \w-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  0.0337
_diffrn_reflns_av_sigmaI/netI    0.0526
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            5203
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.12
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.392
_exptl_absorpt_correction_T_max  0.9757
_exptl_absorpt_correction_T_min  0.8935
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Sheldrick, 2004)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             260
_exptl_crystal_size_max          0.366
_exptl_crystal_size_mid          0.178
_exptl_crystal_size_min          0.062
_refine_diff_density_max         0.542
_refine_diff_density_min         -0.194
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         2308
_refine_ls_number_restraints     160
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1070
_refine_ls_R_factor_gt           0.0697
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0909P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1500
_refine_ls_wR_factor_ref         0.1699
_reflns_number_gt                1473
_reflns_number_total             2308
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060953rsi20061016_061859.cif
_cod_data_source_block           03ATC231
_cod_database_code               4072697