Solvothermal synthesis of [Ni(C4H13N3)2]2Sb4S8: the first compound with a cyclic [Sb4S8]4− anion
Bensch, Wolfgang; Näther, Christian; Stähler, Ralph; Chemical Communications  (2001) 477–; doi:10.1039/b009583o

data_7114915
_publ_section_title
;
 Solvothermal synthesis of [Ni(C4H13N3)2]2Sb4S8: the first compound with a
 cyclic [Sb4S8]4&#x2212; anion
;
_journal_issue                   5
_journal_name_full               'Chemical Communications'
_journal_page_first              477
_journal_paper_doi               10.1039/b009583o
_journal_year                    2001
_chemical_formula_sum            'C16 H52 N12 Ni2 S8 Sb4'
_chemical_formula_weight         1273.60
_chemical_name_systematic
;
Bis[bis(diethylenetriamine)nickel(ii)]Bis[cyclo-octasulfido-
tetraantimonate(iii)]
;
_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                92.299(9)
_cell_angle_beta                 91.058(8)
_cell_angle_gamma                105.735(9)
_cell_formula_units_Z            2
_cell_length_a                   9.0249(6)
_cell_length_b                   12.7597(10)
_cell_length_c                   18.0367(13)
_cell_measurement_temperature    293(2)
_cell_volume                     1996.6(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.497
_diffrn_measured_fraction_theta_max 0.497
_diffrn_measurement_device_type
'STOE Imaging Plate Diffraction System (IPDS)'
_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  0.0536
_diffrn_reflns_av_sigmaI/netI    0.0476
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            7840
_diffrn_reflns_theta_full        25.94
_diffrn_reflns_theta_max         25.94
_diffrn_reflns_theta_min         2.05
_diffrn_standards_decay_%        negligible
_exptl_absorpt_coefficient_mu    4.040
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'STOE X-SHAPE (STOE & CIE, 1997, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.118
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       squares
_exptl_crystal_F_000             1240
_refine_diff_density_max         0.734
_refine_diff_density_min         -0.518
_refine_diff_density_rms         0.093
_refine_ls_extinction_coef       0.0030(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         3871
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0474P)^2^+0.2693P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0775
_refine_ls_wR_factor_ref         0.0814
_reflns_number_gt                3182
_reflns_number_total             3871
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b009583o.txt
_cod_data_source_block           rs125
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7114915