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_4501341
_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         '3(C10 H30 N6 Ni), S12 Sb6'
_chemical_formula_sum            'C30 H90 N18 Ni3 S12 Sb6'
_chemical_formula_weight         1994.55
_chemical_name_common            '[Ni(aepa)2]3Sb6S12'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                120.00
_cell_formula_units_Z            6
_cell_length_a                   22.1486(11)
_cell_length_b                   22.1486(11)
_cell_length_c                   23.6629(13)
_cell_measurement_reflns_used    5411
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.05
_cell_measurement_theta_min      2.29
_cell_volume                     10052.9(9)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0377
_diffrn_reflns_av_sigmaI/netI    0.0207
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            32787
_diffrn_reflns_theta_full        28.05
_diffrn_reflns_theta_max         28.05
_diffrn_reflns_theta_min         2.29
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.615
_exptl_absorpt_correction_T_max  0.7167
_exptl_absorpt_correction_T_min  0.5687
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-Shape (STOE & CIE, 1998)'
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    1.977
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polyhedrons
_exptl_crystal_F_000             5868
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.028
_refine_diff_density_min         -1.121
_refine_diff_density_rms         0.144
_refine_ls_extinction_coef       0.00060(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   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         5411
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0380
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0633P)^2^+27.3961P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0974
_refine_ls_wR_factor_ref         0.1028
_reflns_number_gt                4471
_reflns_number_total             5411
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg201122e_si_001.cif
_cod_data_source_block           bes601
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               4501341