Bis{μ-3,3'-(1,3,4-thiadiazole-2,5-diyldithio)bis[pentanedionato(1{-})]}bis[diaquanickel(II)] dimethylformamide disolvate trihydrate
Jian, Fang-Fang; Han, Song-Jiang; Acta Crystallographica Section E 65 (2009) m207–; doi:10.1107/S1600536808043699

data_2220679
_publ_section_title
;Bis{\m-3,3'-(1,3,4-thiadiazole-2,5-diyldithio)bis[pentanedionato(1{-})]}bis[diaquanickel(II)]
 dimethylformamide disolvate trihydrate
;
_journal_coeditor_code           AT2698
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m207
_journal_paper_doi               10.1107/S1600536808043699
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac
'[Ni2 (C12 H12 N2 O4 S3) (H2 O)4], 2C3 H7 N O, 3H2 O'
_chemical_formula_moiety
'C24 H32 N4 Ni2 O12 S6, 2(C3 H7 N O), 3(H2 O)'
_chemical_formula_sum            'C30 H52 N6 Ni2 O17 S6'
_chemical_formula_weight         1078.56
_chemical_melting_point          554.6
_chemical_name_systematic
;
bis{\m-3,3'-(1,3,4-thiadiazole-2,5-
diyldithio)bis[pentanedionato(1-)]}bis[diaquanickel(II)]
dimethylformamide disolvate trihydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                102.30(3)
_cell_angle_beta                 107.210(10)
_cell_angle_gamma                116.26(3)
_cell_formula_units_Z            1
_cell_length_a                   10.582(2)
_cell_length_b                   11.4690(10)
_cell_length_c                   12.136(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      4
_cell_volume                     1155.6(6)
_computing_cell_refinement       'CAD-4 Software (Enraf--Nonius, 1989)'
_computing_data_collection       'CAD-4 Software (Enraf--Nonius, 1989)'
_computing_data_reduction        'CAD-4 Software (Enraf--Nonius, 1989)'
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 2008)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Enraf--Nonius CAD-4'
_diffrn_measurement_method       \w
_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  0.0127
_diffrn_reflns_av_sigmaI/netI    0.0245
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6130
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.92
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 100
_diffrn_standards_interval_time  0
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.158
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             562
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.465
_refine_diff_density_min         -0.602
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         4039
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0349
_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^)+(0.0451P)^2^+0.9813P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0897
_refine_ls_wR_factor_ref         0.0946
_reflns_number_gt                3498
_reflns_number_total             4039
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            at2698.cif
_cod_data_source_block           I
_cod_database_code               2220679
_cod_database_fobs_code          2220679