From Zero- to Three-Dimensional Thioantimonates: [Ni(aepa)2]3Sb6S12(aepa = C5H15N3=N-(aminoethyl)-1,3-propandiamine), Containing the Unique [Sb6S12]6‒Cyclic Anion, [Ni(aepa)2]6(Sb3S6)2(SO4)3·2H2O, with Isolated [Sb3S6]3‒anions and [Ni(aepa)2]Sb4S7, Characterized by a Three-Dimensional Network Structure
Seidlhofer, Beatrix; Djamil, John; Näther, Christian; Bensch, Wolfgang; Crystal Growth & Design 11 (2011) 5554–; doi:10.1021/cg201122e

data_4501342
_publ_section_title
;
 From Zero- to Three-Dimensional Thioantimonates: [Ni(aepa)2]3Sb6S12(aepa
 = C5H15N3=N-(aminoethyl)-1,3-propandiamine), Containing the Unique
 [Sb6S12]6--Cyclic Anion, [Ni(aepa)2]6(Sb3S6)2(SO4)3&#x00B7;2H2O, with
 Isolated [Sb3S6]3--anions and [Ni(aepa)2]Sb4S7, Characterized by a
 Three-Dimensional Network Structure
;
_journal_issue                   12
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              5554
_journal_paper_doi               10.1021/cg201122e
_journal_volume                  11
_journal_year                    2011
_chemical_formula_moiety         '6(C10 H30 N6 Ni), 3(O4 S), 2(S6 Sb3), O2'
_chemical_formula_sum            'C60 H180 N36 Ni6 O14 S15 Sb6'
_chemical_formula_weight         3198.09
_chemical_name_common            '[Ni(aepa)2]6(Sb3S6)2(SO4)3*2H2O'
_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                73.635(7)
_cell_angle_beta                 85.432(7)
_cell_angle_gamma                63.200(7)
_cell_formula_units_Z            1
_cell_length_a                   13.3436(8)
_cell_length_b                   14.1266(9)
_cell_length_c                   18.3991(12)
_cell_measurement_reflns_used    9945
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.12
_cell_volume                     2965.7(4)
_computing_cell_refinement       'STOE-IPDS Program Package'
_computing_data_collection       'STOE-IPDS Program Package'
_computing_data_reduction        'STOE-IPDS Program Package'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'Stoe Imaging Plate Diffraction System'
_diffrn_measurement_method       '\f 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  0.0542
_diffrn_reflns_av_sigmaI/netI    0.0825
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19111
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.12
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.599
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.791
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             1622
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.018
_refine_diff_density_min         -0.662
_refine_diff_density_rms         0.125
_refine_ls_extinction_coef       0.00091(11)
_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   0.935
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     645
_refine_ls_number_reflns         9945
_refine_ls_number_restraints     87
_refine_ls_restrained_S_all      0.940
_refine_ls_R_factor_all          0.0766
_refine_ls_R_factor_gt           0.0406
_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^)+(0.0368P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0753
_refine_ls_wR_factor_ref         0.0850
_reflns_number_gt                6757
_reflns_number_total             9945
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg201122e_si_002.cif
_cod_data_source_block           bes839
_cod_original_cell_volume        2965.7(3)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4501342