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_4302880
_publ_section_title
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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         'C14 H24 Fe N6 S2, B F4'
_chemical_formula_sum            'C14 H24 B F4 Fe N6 S2'
_chemical_formula_weight         483.17
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 98.786(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.5350(3)
_cell_length_b                   12.2605(4)
_cell_length_c                   18.9435(6)
_cell_measurement_temperature    100(2)
_cell_volume                     1959.05(11)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker-Nonius Kappa-CCD'
_diffrn_measurement_method
'629 images at 1.0 deg. stepwise rotation in omega and phi, 110 sec./frame'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode, 50 kV, 80 mA'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_av_sigmaI/netI    0.0327
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            37245
_diffrn_reflns_theta_full        33.16
_diffrn_reflns_theta_max         33.16
_diffrn_reflns_theta_min         2.93
_exptl_absorpt_coefficient_mu    1.033
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.5286
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS Vers. 2006/1, Bruker AXS (2006)'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'opaque parallelepiped'
_exptl_crystal_F_000             996
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.483
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         7433
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0320
_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^)+(0.0288P)^2^+1.0754P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0687
_refine_ls_wR_factor_ref         0.0740
_reflns_number_gt                6176
_reflns_number_total             7433
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900936p_si_002_3.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_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               4302880