Oxalato-Bridged Dinuclear Complexes of Cr(III) and Fe(III): Synthesis, Structure, and Magnetism of [(C2H5)4N]4[MM'(ox)(NCS)8] with MM' = CrCr, FeFe, and CrFe
Smaïl Triki; Florence Bérézovsky; Jean Sala Pala; Eugenio Coronado; Carlos J. Gómez-García; Juan Modesto Clemente; Amédée Riou; Philippe Molinié; Inorganic Chemistry 39 (2000) 3771–3776; doi:10.1021/ic990439w

data_4321277
_publ_contact_author
;
Triki Smail
UMR CNRS 6521, Chimie, Electrochimie Moleculaire 
et Chimie Analytique, Universite de Bretagne 
Occidentale, 29285 Brest Cedex, France.
;
_publ_contact_author_email       triki@univ-brest.fr
_publ_contact_author_fax         '(33) 2 98 01 65 94'
_publ_contact_author_phone       '(33) 2 98 01 61 46'
_publ_section_title
;
 Oxalato-Bridged Dinuclear Complexes of Cr(III) and Fe(III): Synthesis,
 Structure, and Magnetism of [(C2H5)4N]4[MM'(ox)(NCS)8] with MM' = CrCr,
 FeFe, and CrFe
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3771
_journal_page_last               3776
_journal_paper_doi               10.1021/ic990439w
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C21 H40 Cr0.5 Fe0.5 N6 O2 S4'
_chemical_formula_weight         590.76
_chemical_name_systematic
; 

 ? 

;
_space_group_IT_number           64
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2ac 2'
_symmetry_space_group_name_H-M   'C m c a'
_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            8
_cell_length_a                   16.664(7)
_cell_length_b                   13.575(6)
_cell_length_c                   28.386(8)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11.94
_cell_measurement_theta_min      4.85
_cell_volume                     6421(4)
_computing_cell_refinement       'CAD4 (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 (Enraf Nonius, 1994)'
_computing_data_reduction        MolEN
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.469
_diffrn_measured_fraction_theta_max 0.469
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.2488
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3130
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         2.06
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.699
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2504
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.327
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.910
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         2928
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.910
_refine_ls_R_factor_all          0.3189
_refine_ls_R_factor_gt           0.0878
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1387P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2156
_refine_ls_wR_factor_ref         0.3157
_reflns_number_gt                794
_reflns_number_total             2928
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic990439w.cif
_cod_data_source_block           C21H40Cr0.50Fe0.50N6O2S4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'None' changed to
'none' according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1387P)^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^)+(0.1387P)^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_formula_sum        'C21 H40 Cr0.50 Fe0.50 N6 O2 S4'
_cod_database_code               4321277