Octahedral Monodithiolene Complexes of Iron: Characterization of S,S'-Coordinated Dithiolate(1-) π Radical Monoanions: A Spectroscopic and Density Functional Theoretical Investigation
Carsten Milsmann; Goutam Kumar Patra; Eckhard Bill; Thomas Weyhermüller; Serena DeBeer George; Karl Wieghardt; Inorganic Chemistry 48 (2009) 7430–7445; doi:10.1021/ic900936p

data_4302878
_publ_section_title
;
Octahedral Monodithiolene Complexes of Iron: Characterization
of S,S'-Coordinated Dithiolate(1-) \p Radical Monoanions: A
Spectroscopic and Density Functional Theoretical Investigation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7430
_journal_page_last               7445
_journal_paper_doi               10.1021/ic900936p
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C15 H34 Fe N5 S2, 2(C F3 O3 S), C2 H3 N'
_chemical_formula_sum            'C19 H37 F6 Fe N6 O6 S4'
_chemical_formula_weight         743.64
_chemical_name_systematic
; 
 ? 
;
_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                89.832(2)
_cell_angle_beta                 82.675(2)
_cell_angle_gamma                83.205(2)
_cell_formula_units_Z            2
_cell_length_a                   9.1969(3)
_cell_length_b                   11.6996(4)
_cell_length_c                   14.5177(4)
_cell_measurement_temperature    100(2)
_cell_volume                     1538.36(8)
_computing_cell_refinement       'Bruker AXS Collect Software'
_computing_data_collection       'Bruker AXS Collect Software'
_computing_data_reduction        'Bruker AXS Collect Software'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method
'828 images at 1.0 deg. stepwise rotation in omega and phi, 15 sec./frame'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_av_sigmaI/netI    0.0485
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            37258
_diffrn_reflns_theta_full        32.50
_diffrn_reflns_theta_max         32.50
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    0.843
_exptl_absorpt_correction_T_max  0.9512
_exptl_absorpt_correction_T_min  0.8631
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2006/1, Bruker AXS'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'transparent parallelepiped'
_exptl_crystal_F_000             770
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.562
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         11108
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0330
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+0.5280P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0775
_refine_ls_wR_factor_ref         0.0826
_reflns_number_gt                9160
_reflns_number_total             11108
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900936p_si_002_1.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Multi-Scan' changed to
'multi-scan' 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_enum 1527 2010-12-29 10:47:43Z saulius 
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_cod_database_code               4302878