Ni(II) and hs-Fe(II) Complexes of a Paramagnetic Thiazyl Ligand, and Decomposition Products of the Iron Complex, Including an Fe(III) Tetramer
Nigel G. R. Hearns; Elisabeth M. Fatila; Rodolphe Clérac; Michael Jennings; Kathryn E. Preuss; Inorganic Chemistry 47 (2008) 10330–10341; doi:10.1021/ic800749b

data_4305815
_publ_contact_author_address
; 
Department of Chemistry, University of Guelph, 
50 Stone Road East, Guelph, Ontario N1G 2W1, Canada
;
_publ_contact_author_email       kpreuss@uoguelph.ca
_publ_contact_author_name        'Professor Kathryn E. Preuss'
_publ_section_title
;
Ni(II) and hs-Fe(II) Complexes of a Paramagnetic Thiazyl Ligand, and
Decomposition Products of the Iron Complex, Including an Fe(III) Tetramer
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10330
_journal_page_last               10341
_journal_paper_doi               10.1021/ic800749b
_journal_volume                  47
_journal_year                    2008
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C16 H6 F12 Fe N3 O4 S2'
_chemical_formula_sum            'C16 H6 F12 Fe N3 O4 S2'
_chemical_formula_weight         652.21
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.8809(6)
_cell_length_b                   16.6466(9)
_cell_length_c                   15.3774(12)
_cell_measurement_reflns_used    85562
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.04
_cell_volume                     2273.3(3)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001)'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 2001)'
_computing_publication_material  SHELXTL/PC
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       '\f scans, and \w scans with \k offsets'
_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  0.0680
_diffrn_reflns_av_sigmaI/netI    0.0259
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18248
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.60
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.976
_exptl_absorpt_correction_T_max  0.9087
_exptl_absorpt_correction_T_min  0.6817
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO-SMN (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.906
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1284
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.222
_refine_diff_density_min         -0.571
_refine_diff_density_rms         0.110
_refine_ls_abs_structure_details
'Flack H D (1983), 1654 Friedelpairs, Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.50(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     413
_refine_ls_number_reflns         3700
_refine_ls_number_restraints     651
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0821
_refine_ls_R_factor_gt           0.0715
_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^)+(0.1006P)^2^+9.7140P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1923
_refine_ls_wR_factor_ref         0.2028
_reflns_number_gt                3263
_reflns_number_total             3700
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic800749b_si_001_3.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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 
;
_cod_database_code               4305815