Ionothermal Synthesis of Four New Nickel Thiophosphate Anions: [Ni(P2S8)2]2-, [Ni(P3S9)(P2S8)]3-, [Ni(P3S9)2]4-, and [(NiP3S8)4(PS4)]7-
Jason A. Cody; Kenneth B. Finch; Gilbert J. Reynders; Grant C. B. Alexander; Hyung G. Lim; Christian Näther; Wolfgang Bensch; Inorganic Chemistry 51 (2012) 13357–13362; doi:10.1021/ic302112g

data_4331342
_publ_section_title
;
 Ionothermal Synthesis of Four New Nickel Thiophosphate Anions:
 [Ni(P2S8)2]2-, [Ni(P3S9)(P2S8)]3-, [Ni(P3S9)2]4-, and [(NiP3S8)4(PS4)]7-
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              13357
_journal_page_last               13362
_journal_paper_doi               10.1021/ic302112g
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C18 H33 N6 Ni P5 S17'
_chemical_formula_weight         1092.08
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 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            12
_cell_length_a                   11.8394(2)
_cell_length_b                   20.0693(3)
_cell_length_c                   56.7184(13)
_cell_measurement_temperature    293(2)
_cell_volume                     13476.8(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0358
_diffrn_reflns_av_sigmaI/netI    0.0289
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            42455
_diffrn_reflns_theta_full        19.48
_diffrn_reflns_theta_max         19.48
_diffrn_reflns_theta_min         1.08
_exptl_absorpt_coefficient_mu    1.425
_exptl_absorpt_correction_T_max  0.8621
_exptl_absorpt_correction_T_min  0.6338
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-red and X-shape (STOE&CIE)'
_exptl_crystal_density_diffrn    1.615
_exptl_crystal_F_000             6696
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.759
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.010(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     910
_refine_ls_number_reflns         11626
_refine_ls_number_restraints     234
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0444
_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^)+(0.0788P)^2^+13.1586P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1196
_refine_ls_wR_factor_ref         0.1222
_reflns_number_gt                10655
_reflns_number_total             11626
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302112g_si_001_3.cif
_cod_data_source_block           2_Ni(P2S8)(P3S9)
_cod_database_code               4331342