The new thioantimonate(V) (C~3~H~10~N)[NiSbS~4~(C~6~H~18~N~4~)]
Ralph Stähler; Wolfgang Bensch; Acta Crystallographica Section C 58 (2002) m537–m538; doi:10.1107/S0108270102017754

data_2013008
_publ_section_title
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 The new thioantimonate(V) (C~3~H~10~N)[NiSbS~4~(C~6~H~18~N~4~)]
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_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m537
_journal_page_last               m538
_journal_paper_doi               10.1107/S0108270102017754
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          '(C3 H10 N) [Ni Sb S4 (C6 H18 N4)]'
_chemical_formula_moiety         'C3 H10 N + , C6 H18 N4 Ni S4 Sb - '
_chemical_formula_sum            'C9 H28 N5 Ni S4 Sb'
_chemical_formula_weight         515.06
_chemical_name_systematic
;
propylammonium tris(2-aminoethyl)amine-1\k^4^N-di-\m-thio-1:2\k^4^S-dithio-
2\k^2^S-antimony(V)nickel(II)
;
_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           SHELXL97
_cell_angle_alpha                63.98(3)
_cell_angle_beta                 84.49(3)
_cell_angle_gamma                82.26(3)
_cell_formula_units_Z            2
_cell_length_a                   7.5707(15)
_cell_length_b                   11.303(2)
_cell_length_c                   12.605(3)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29
_cell_measurement_theta_min      20
_cell_volume                     959.6(4)
_computing_cell_refinement       DIF4
_computing_data_collection       'DIF4 (Stoe & Cie, 1992)'
_computing_data_reduction        'REDU4 (Stoe & Cie, 1992)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'CIFTAB in SHELXL97'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Philips PW1100 four-circle'
_diffrn_measurement_method       \w/\q
_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  0.013
_diffrn_reflns_av_sigmaI/netI    0.025
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4967
_diffrn_reflns_theta_full        28.02
_diffrn_reflns_theta_max         28.02
_diffrn_reflns_theta_min         2.72
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.821
_exptl_absorpt_correction_T_max  0.720
_exptl_absorpt_correction_T_min  0.513
_exptl_absorpt_correction_type   '\y scan'
_exptl_absorpt_process_details
'[X-SHAPE (Stoe & Cie, 1998) and X-RED (Stoe & Cie, 1998)]'
_exptl_crystal_colour            turquoise
_exptl_crystal_density_diffrn    1.782
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.71
_refine_diff_density_min         -0.47
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         4625
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.031
_refine_ls_R_factor_gt           0.019
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0217P)^2^+0.3866P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.047
_refine_ls_wR_factor_ref         0.050
_reflns_number_gt                3940
_reflns_number_total             4625
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            av1121.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
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_cod_original_cell_volume        959.7(3)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2013008
_cod_database_fobs_code          2013008