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_4307475
_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 Cu F12 N3 O4 S2'
_chemical_formula_sum            'C16 H6 Cu F12 N3 O4 S2'
_chemical_formula_weight         659.93
_chemical_name_systematic
;
[4-(2-pyridyl)-1,2,4,5-dithiadiazolyl]-bis(hexafluoroacetylacetonate)
copper(II) 
;
_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                 97.975(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   9.3999(19)
_cell_length_b                   30.749(6)
_cell_length_c                   15.537(3)
_cell_measurement_reflns_used    5198
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.09
_cell_measurement_theta_min      2.56
_cell_volume                     4447.3(15)
_computing_cell_refinement       'SAINT 6.22 (Bruker, 2001)'
_computing_data_collection       'SMART 5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT 6.22 (Bruker, 2001)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       /w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1094
_diffrn_reflns_av_sigmaI/netI    0.1462
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            39738
_diffrn_reflns_theta_full        28.24
_diffrn_reflns_theta_max         28.24
_diffrn_reflns_theta_min         1.48
_diffrn_standards_decay_%        <0.1
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.302
_exptl_absorpt_correction_T_max  0.922
_exptl_absorpt_correction_T_min  0.632
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.971
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2592
_exptl_crystal_size_max          0.246
_exptl_crystal_size_mid          0.144
_exptl_crystal_size_min          0.062
_refine_diff_density_max         1.731
_refine_diff_density_min         -0.867
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     662
_refine_ls_number_reflns         10536
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1625
_refine_ls_R_factor_gt           0.0785
_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^)+(0.0987P)^2^+14.6270P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1863
_refine_ls_wR_factor_ref         0.2201
_reflns_number_gt                5739
_reflns_number_total             10536
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0619456-file001_1.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4307475