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_4077572
_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            'C8 H12 N2 O S2'
_chemical_formula_weight         216.32
_chemical_name_common            'Compound 3'
_chemical_name_systematic
; 
N',N'-Dimethylhydrazono-1-(1,3-dithiolane-2-yliden)propanone
;
_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                 110.43(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.335(1)
_cell_length_b                   11.940(1)
_cell_length_c                   11.324(3)
_cell_measurement_reflns_used    29
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.50
_cell_measurement_theta_min      5.00
_cell_volume                     1056.1(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.949
_diffrn_measured_fraction_theta_max 0.949
_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  0.0333
_diffrn_reflns_av_sigmaI/netI    0.0401
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            1994
_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    0.468
_exptl_absorpt_correction_T_max  0.782
_exptl_absorpt_correction_T_min  0.730
_exptl_absorpt_correction_type   psi-scans
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             456
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.491
_refine_diff_density_min         -0.342
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       0.026(3)
_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   1.040
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     119
_refine_ls_number_reflns         1861
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0491
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0584P)^2^+0.7307P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1183
_refine_ls_wR_factor_ref         0.1346
_reflns_number_gt                1359
_reflns_number_total             1861
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0004702.cif
_cod_data_source_block           ns1
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0584P)^2^+0.7307P] 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^)+(0.0584P)^2^+0.7307P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4077572