Synthesis and Characterization of Novel Iron(0) Complexes Derived from α,β-Unsaturated-Ketone Analogues with β-Positioned Heteroatoms Containing Covalent and Coordination Bonds
Ortega-Jiménez, Fernando; Ortega-Alfaro, M. Carmen; López-Cortés, José G.; Gutiérrez-Pérez, René; Toscano, Rubén A.; Velasco-Ibarra, Luis; Peña-Cabrera, Eduardo; Alvarez-Toledano, Cecilio; Organometallics 19 (2000) 4127–; doi:10.1021/om0004702

data_4077576
_publ_section_title
;
 Synthesis and Characterization of Novel Iron(0) Complexes Derived from
 \a,\b-Unsaturated-Ketone Analogues with \b-Positioned Heteroatoms
 Containing Covalent and Coordination Bonds
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              4127
_journal_paper_doi               10.1021/om0004702
_journal_volume                  19
_journal_year                    2000
_chemical_formula_sum            'C14 H12 Fe2 N2 O7 S2'
_chemical_formula_weight         496.08
_chemical_name_common            'Compound 9'
_chemical_name_systematic
; 
Hexacarbonyl-\mN,\sO,\sC-[N',N'-Dimethylhydrazono-1-(1,3-dithiolane-2-yliden)
propanone]diiron(0)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.00(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.072(6)
_cell_length_b                   9.680(2)
_cell_length_c                   13.174(3)
_cell_measurement_reflns_used    32
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.50
_cell_measurement_theta_min      5.00
_cell_volume                     1960.0(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.873
_diffrn_measured_fraction_theta_max 0.873
_diffrn_measurement_device_type  'Siemens P4/PC diffractometer'
_diffrn_measurement_method       \q:2\q
_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  0.0584
_diffrn_reflns_av_sigmaI/netI    0.1042
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3380
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.50
_diffrn_standards_decay_%        3
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.730
_exptl_absorpt_correction_T_max  0.947
_exptl_absorpt_correction_T_min  0.654
_exptl_absorpt_correction_type   psi-scans
_exptl_crystal_colour            'deep red'
_exptl_crystal_density_diffrn    1.681
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.892
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.127
_refine_ls_extinction_coef       0.0035(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         3220
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.1191
_refine_ls_R_factor_gt           0.0618
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0775P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1530
_refine_ls_wR_factor_ref         0.1868
_reflns_number_gt                1936
_reflns_number_total             3220
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0004702.cif
_cod_data_source_block           a9962s
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0775P)^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^)+(0.0775P)^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        1960.0(9)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4077576