2,2',2''-Nitrilotris(ethylammonium) tetrathioantimonate
Poisot, Martha; Näther, Christian; Bensch, Wolfgang; Acta Crystallographica Section E 63 (2007) m1751–m1752; doi:10.1107/S160053680702394X

data_2214012
_publ_section_title
;
 2,2',2''-Nitrilotris(ethylammonium) tetrathioantimonate
;
_journal_coeditor_code           ZL2025
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1751
_journal_page_last               m1752
_journal_paper_doi               10.1107/S160053680702394X
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '(C6 H21 N4) [Sb S4]'
_chemical_formula_moiety         'C6 H21 N4 3+, S4 Sb 3-'
_chemical_formula_sum            'C6 H21 N4 S4 Sb'
_chemical_formula_weight         399.26
_chemical_name_systematic
;
2,2',2''-Nitrilotris(ethylammonium) tetrathioantimonate
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 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            8
_cell_length_a                   19.7872(13)
_cell_length_b                   10.8571(10)
_cell_length_c                   13.5055(8)
_cell_measurement_reflns_used    132
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      13
_cell_volume                     2901.4(4)
_computing_cell_refinement       DIF4
_computing_data_collection       'DIF4 (Stoe & Cie, 1992)'
_computing_data_reduction        'REDU4 (Stoe & Cie, 1992)'
_computing_molecular_graphics
;
XP in SHELXTL (Bruker, 1998) and 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  'Stoe AEDII'
_diffrn_measurement_method       'Phi 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  0.0231
_diffrn_reflns_av_sigmaI/netI    0.0281
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       1
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6750
_diffrn_reflns_theta_full        27.01
_diffrn_reflns_theta_max         27.01
_diffrn_reflns_theta_min         1.88
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  '2 h'
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    2.456
_exptl_absorpt_correction_T_max  0.772
_exptl_absorpt_correction_T_min  0.738
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(X-Shape; Stoe & Cie, 1998)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.828
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.878
_refine_diff_density_min         -0.551
_refine_ls_abs_structure_details 'Flack (1983), 544 Friedel pairs'
_refine_ls_abs_structure_Flack   0.04(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         3571
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0248
_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^)+(0.0261P)^2^+3.7053P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0611
_refine_ls_wR_factor_ref         0.0650
_reflns_number_gt                2898
_reflns_number_total             3571
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            zl2025.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P ca21'
_cod_database_code               2214012
_cod_database_fobs_code          2214012