Synthesis and crystal structure of decacarbonyl(μ~3~-3,7-dithianonane-1,9-dithiolato)bis(μ~2~-propane-1,3-dithiolato)nickel(II)tetrairon(II) dichloromethane disolvate
Ren, Gan; Sang, Ge; Acta Crystallographica Section E 74 (2018) 328–331; doi:10.1107/S2056989018001731

data_2242385
_publ_section_title
;
 Synthesis and crystal structure of
 decacarbonyl(\m~3~-3,7-dithianonane-1,9-dithiolato)bis(\m~2~-propane-1,3-dithiolato)nickel(II)tetrairon(II)
 dichloromethane disolvate
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              328
_journal_page_last               331
_journal_paper_doi               10.1107/S2056989018001731
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac
'[Fe4 Ni (C3 H6 S2)2 (C7 H14 S4) (C O)10], 2C H2 Cl2'
_chemical_formula_moiety         'C23 H26 Fe4 Ni O10 S8, 2(C H2 Cl2)'
_chemical_formula_sum            'C25 H30 Cl4 Fe4 Ni O10 S8'
_chemical_formula_weight         1170.88
_chemical_name_common            Fe4NiS6
_chemical_name_systematic
'Decacarbonyl(\m~3~-3,7-dithianonane-1,9-dithiolato)bis(\m~2~-propane-1,3-dithiolato)nickel(II)tetrairon(II) dichloromethane disolvate'
_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                77.860(4)
_cell_angle_beta                 67.570(4)
_cell_angle_gamma                64.036(4)
_cell_formula_units_Z            2
_cell_length_a                   12.4340(8)
_cell_length_b                   13.9981(10)
_cell_length_c                   14.4912(9)
_cell_measurement_reflns_used    6326
_cell_measurement_temperature    243(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.93
_cell_volume                     2093.3(3)
_computing_cell_refinement
;
SAINT-Plus (Bruker, 2007)
;
_computing_data_collection
;
APEX2 (Bruker, 2007)
;
_computing_data_reduction
;
SAINT-Plus (Bruker, 2007)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008) and Mercury (Macrae <i>et al.</i>,
2008)
;
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008), PLATON (Spek, 2009) and
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      243(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEXII area detector'
_diffrn_measurement_method       'phi and omega 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  0.0337
_diffrn_reflns_av_sigmaI/netI    0.0394
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20488
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.93
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.497
_exptl_absorpt_correction_T_max  0.6351
_exptl_absorpt_correction_T_min  0.4350
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2007)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.858
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.940
_refine_diff_density_min         -0.592
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     497
_refine_ls_number_reflns         7352
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0319
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0322P)^2^+1.0504P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0685
_refine_ls_wR_factor_ref         0.0751
_reflns_number_gt                5928
_reflns_number_total             7352
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            su5420sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        2093.3(2)
_cod_database_code               2242385
_cod_database_fobs_code 2242385