Tuning the oxidation state and magnetic and coordination behaviour of iron and cobalt complexes by O/S variation in mono-thio and dithio-oxamide chelating ligands
Pilia, Luca; Espa, Davide; Concas, Giorgio; Congiu, Francesco; Marchiò, Luciano; Laura Mercuri, M.; Serpe, Angela; Deplano, Paola; New J. Chem. 39 (2015) 4716–; doi:10.1039/C5NJ00425J

data_7054758
_publ_section_title
;
 Tuning the oxidation state and magnetic and coordination behaviour of
 iron and cobalt complexes by O/S variation in mono-thio and
 dithio-oxamide chelating ligands
;
_journal_issue                   6
_journal_name_full               'New J. Chem.'
_journal_page_first              4716
_journal_paper_doi               10.1039/C5NJ00425J
_journal_volume                  39
_journal_year                    2015
_chemical_formula_moiety         'C18 H30 Fe N6 S6 2+, 2(B F4 1-)'
_chemical_formula_sum            'C18 H30 B2 F8 Fe N6 S6'
_chemical_formula_weight         752.31
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2014-12-05 deposited with the CCDC.
2015-03-18 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 134.54(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.662(5)
_cell_length_b                   11.130(3)
_cell_length_c                   18.004(4)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      16.81
_cell_measurement_theta_min      6.12
_cell_volume                     3236.7(17)
_computing_cell_refinement       'local program'
_computing_data_collection       'local program'
_computing_data_reduction        'local program'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    Sir97
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Philips PW 1100 diffractometer'
_diffrn_measurement_method       theta-2-theta
_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  0.0286
_diffrn_reflns_av_sigmaI/netI    0.1571
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3258
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.07
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 100
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    0.921
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.944
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
local program based on Walker & Stuart,
(a) Walker, N.; Stuart, D. Acta Crystallogr., Sect. A 1983, 39, 158;
(b) Ugozzoli, F. Comput. Chem. 1987, 11, 109
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.534
_refine_diff_density_min         -0.385
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     189
_refine_ls_number_reflns         3160
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1700
_refine_ls_R_factor_gt           0.0482
_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^)+(0.0001P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0592
_refine_ls_wR_factor_ref         0.0711
_reflns_number_gt                1188
_reflns_number_total             3160
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5nj00425j1.cif
_cod_data_source_block           feesa_compound_1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3105 2015-03-04 15:46:00Z robertas 

 Adding full bibliography for 7054758--7054762.cif.
;
_cod_original_cell_volume        3236.7(13)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7054758