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_4072699
_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         'C15 H16 Fe2 N2 O6 S2'
_chemical_formula_sum            'C15 H16 Fe2 N2 O6 S2'
_chemical_formula_weight         496.12
_chemical_name_systematic
; 
8-Methyl-6,6,10,10,10-pentacarbonyl-9-tert-butylhydrazono-6,10-
diferra-7-oxa-2,5-dithiapentacycle[4.3.0.1^2,5^.0^1,10^.0^6,10^]
decan-7,9-diene
;
_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                97.179(2)
_cell_angle_beta                 94.098(2)
_cell_angle_gamma                113.176(2)
_cell_formula_units_Z            2
_cell_length_a                   7.519(1)
_cell_length_b                   7.918(1)
_cell_length_c                   19.177(1)
_cell_measurement_reflns_used    4122
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      30.84
_cell_measurement_theta_min      2.84
_cell_volume                     1032.2(2)
_computing_cell_refinement       'SMART V 5.625 (Bruker, 1999)'
_computing_data_collection       'SMART V 5.625 (Bruker, 1999)'
_computing_data_reduction        'SAINT V 6.23C (Bruker, 1999)'
_computing_molecular_graphics    'SHELXTL V 6.12 (Sheldrick, 2000)'
_computing_publication_material  'SHELXTL V 6.12 (Sheldrick, 2000)'
_computing_structure_refinement  'SHELXTL V 6.12 (Sheldrick, 2000)'
_computing_structure_solution    'SHELXTL V 6.12 (Sheldrick, 2000)'
_diffrn_ambient_temperature      294(2)
_diffrn_detector_area_resol_mean 0.661
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Smart Apex CCD diffractometer'
_diffrn_measurement_method       '\y and \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  0.0426
_diffrn_reflns_av_sigmaI/netI    0.0457
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12266
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.16
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.639
_exptl_absorpt_correction_T_max  0.9616
_exptl_absorpt_correction_T_min  0.7463
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Sheldrick, 2004)'
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    1.596
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.186
_exptl_crystal_size_mid          0.168
_exptl_crystal_size_min          0.024
_refine_diff_density_max         0.507
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     279
_refine_ls_number_reflns         3635
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0501
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0598P)^2^+0.2385P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1087
_refine_ls_wR_factor_ref         0.1161
_reflns_number_gt                2910
_reflns_number_total             3635
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060953rsi20061016_062004.cif
_cod_data_source_block           217ATC04
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               4072699