Unusual C-S Bond Cleavage in Hydro(solvo)thermal Reaction That Induces Two Novel Nickel Thiolates: The Crown [Ni16(edt)8S9(S2)]4- with an Unprecedented 12-Membered Ring System and the Cagelike [Ni13(edt)8S4(S2)2]2- with Two Distorted Cores
Hao Jiang; Tianlu Sheng; Songyan Bai; Shengmin Hu; Xin Wang; Ruibiao Fu; Peng Yu; Xintao Wu; Inorganic Chemistry 52 (2013) 12305–12307; doi:10.1021/ic400824f

data_4336504
_publ_section_title
;
 Unusual C-S Bond Cleavage in Hydro(solvo)thermal Reaction That Induces
 Two Novel Nickel Thiolates: The Crown [Ni16(edt)8S9(S2)]4- with an
 Unprecedented 12-Membered Ring System and the Cagelike
 [Ni13(edt)8S4(S2)2]2- with Two Distorted Cores
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12305
_journal_page_last               12307
_journal_paper_doi               10.1021/ic400824f
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C40 H96 N4 Ni16 O0 S27'
_chemical_formula_weight         2438.19
_chemical_name_systematic
; 
 ? 
;
_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                94.533(11)
_cell_angle_beta                 90.21(2)
_cell_angle_gamma                92.358(15)
_cell_formula_units_Z            1
_cell_length_a                   11.499(10)
_cell_length_b                   12.749(12)
_cell_length_c                   13.922(13)
_cell_measurement_reflns_used    5822
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      27.4855
_cell_measurement_theta_min      2.0863
_cell_volume                     2033(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       CCD_Profile_fitting
_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  0.0350
_diffrn_reflns_av_sigmaI/netI    0.0541
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13045
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.34
_exptl_absorpt_coefficient_mu    4.333
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5232
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.992
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1244
_exptl_crystal_size_max          0.1300
_exptl_crystal_size_mid          0.0600
_exptl_crystal_size_min          0.0500
_refine_diff_density_max         2.113
_refine_diff_density_min         -1.197
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    geom
_refine_ls_matrix_type           full
_refine_ls_number_parameters     587
_refine_ls_number_reflns         6912
_refine_ls_number_restraints     1244
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0934
_refine_ls_R_factor_gt           0.0741
_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^)+(0.1378P)^2^+3.5153P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2125
_refine_ls_wR_factor_ref         0.2328
_reflns_number_gt                5184
_reflns_number_total             6912
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400824f_si_002.cif
_cod_data_source_block           a
_cod_database_code               4336504