Design and Synthesis of a 4-(2'-Pyridyl)-1,2,3,5-Dithiadiazolyl Cobalt Complex
Nigel G. R. Hearns; Kathryn E. Preuss; John F. Richardson; Sofi Bin-Salamon; Journal of the American Chemical Society 126 (2004) 9942–9943; doi:10.1021/ja046304t

data_4112847
_publ_section_title
;
 Design and Synthesis of a 4-(2'-Pyridyl)-1,2,3,5-Dithiadiazolyl Cobalt
 Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9942
_journal_page_last               9943
_journal_paper_doi               10.1021/ja046304t
_journal_volume                  126
_journal_year                    2004
_chemical_formula_moiety         'C16 H6 Co F12 N3 O4 S2'
_chemical_formula_sum            'C16 H6 Co F12 N3 O4 S2'
_chemical_formula_weight         655.29
_chemical_melting_point          384(1)
_chemical_name_common            '[4-(2'-pyridyl)-1,2,3,5-DTA]Co(hfac)2'
_chemical_name_systematic
; 
 [4-(2'-pyridine)-1,2,3,5-dithiadiazolyl]Co(hexaflouroacetate)2 
;
_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                   8.8720(2)
_cell_length_b                   16.580(3)
_cell_length_c                   15.119(3)
_cell_measurement_reflns_used    4053
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.79
_cell_measurement_theta_min      2.45
_cell_volume                     2224.0(6)
_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    'SHELXTL 6.12 (Bruker, 2001)'
_computing_publication_material  'SHELXTL 6.12 (Bruker, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-90 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       /w-scans
_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  0.0682
_diffrn_reflns_av_sigmaI/netI    0.0892
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18697
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.04
_diffrn_reflns_theta_min         1.82
_diffrn_standards_decay_%        <0.1
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.091
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.864
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sheldrick, G. M.; SADABS (1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.957
_exptl_crystal_description       plate
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.154
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.015
_refine_diff_density_max         0.458
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.092
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         5148
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0916
_refine_ls_R_factor_gt           0.0522
_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^)+(0.0498P)^2^+1.6976P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1078
_refine_ls_wR_factor_ref         0.1201
_reflns_number_gt                3638
_reflns_number_total             5148
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja046304tsi20040622_042410.cif
_cod_data_source_block           kp03lt
_cod_original_sg_symbol_Hall     P2c-2n
_cod_database_code               4112847