Mn(II) and Cu(II) Complexes of a Dithiadiazolyl Radical Ligand: Monomer/Dimer Equilibria in Solution
James Britten; Nigel G. R. Hearns; Kathryn E. Preuss; John F. Richardson; Sofi Bin-Salamon; Inorganic Chemistry 46 (2007) 3934–3945; doi:10.1021/ic0619456

data_4307476
_publ_contact_author_address
;
Department of Chemistry
University of Guelph
Guelph, Ontario N1G 2W1, Canada
;
_publ_contact_author_email       kpreuss@uoguelph.ca
_publ_contact_author_fax         '001 519 766-1499'
_publ_contact_author_name        'Professor Dr. Kathryn E. Preuss'
_publ_contact_author_phone       '001 519 824-4120 x56711'
_publ_section_title
;
Mn(II) and Cu(II) Complexes of a Dithiadiazolyl Radical Ligand:
Monomer/Dimer Equilibria in Solution
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3934
_journal_page_last               3945
_journal_paper_doi               10.1021/ic0619456
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C16 H6 F12 Mn N3 O4 S2'
_chemical_formula_sum            'C16 H6 F12 Mn N3 O4 S2'
_chemical_formula_weight         651.32
_chemical_name_systematic
; 
[4-(2-pyridyl)-1,2,4,5-dithiadiazolyl]-bis(hexafluoroacetylacetonate)
manganese(II) 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 116.190(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.663(16)
_cell_length_b                   17.815(17)
_cell_length_c                   17.467(17)
_cell_measurement_temperature    100(2)
_cell_volume                     4653(8)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Kappa-CCD server software (Nonius, 1997)'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  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  0.1540
_diffrn_reflns_av_sigmaI/netI    0.1737
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            38769
_diffrn_reflns_theta_full        26.55
_diffrn_reflns_theta_max         26.55
_diffrn_reflns_theta_min         1.36
_exptl_absorpt_coefficient_mu    0.873
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            bright-red
_exptl_crystal_density_diffrn    1.860
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2560
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.415
_refine_diff_density_min         -1.152
_refine_diff_density_rms         0.118
_refine_ls_extinction_coef       0.00056(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     672
_refine_ls_number_reflns         9592
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.1868
_refine_ls_R_factor_gt           0.0835
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0666P)^2^+9.2061P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1556
_refine_ls_wR_factor_ref         0.1901
_reflns_number_gt                4746
_reflns_number_total             9592
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0619456-file001_2.cif
_cod_data_source_block           2
_cod_database_code               4307476