A low-temperature refinement of tris[<i>N</i>,<i>N</i>'-bis(2-hydroxyethyl)dithiocarbamato-κ^2^<i>S</i>,<i>S</i>']antimony(III)
Tiekink, Edward R. T.; Young, David J.; Acta Crystallographica Section E 62 (2006) m1887–m1889; doi:10.1107/S1600536806027061

data_2209959
_publ_section_title
;A low-temperature refinement of
 tris[<i>N</i>,<i>N</i>'-bis(2-hydroxyethyl)dithiocarbamato-\k^2^<i>S</i>,<i>S</i>']antimony(III)
;
_journal_coeditor_code           NG2043
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1887
_journal_page_last               m1889
_journal_paper_doi               10.1107/S1600536806027061
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Sb (C5 H10 N1 O2 S2)3]'
_chemical_formula_moiety         'C15 H30 N3 O6 S6 Sb'
_chemical_formula_sum            'C15 H30 N3 O6 S6 Sb'
_chemical_formula_weight         662.53
_chemical_name_systematic
;
tris[N,N'-bis(2-hydroxyethyl)dithiocarbamato-\k^2^S,S']antimony(III)
;
_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                104.422(4)
_cell_angle_beta                 105.294(4)
_cell_angle_gamma                94.445(3)
_cell_formula_units_Z            2
_cell_length_a                   9.942(2)
_cell_length_b                   11.011(2)
_cell_length_c                   12.458(3)
_cell_measurement_reflns_used    5129
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.9
_cell_volume                     1259.0(5)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku/MSC, 2005)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics
'ORTEPII (Johnson, 1976) and DIAMOND (Crystal Impact, 2006)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>,  1994)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  AFC12\K/SATURN724
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.033
_diffrn_reflns_av_sigmaI/netI    0.018
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_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            31926
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         2.9
_diffrn_standards_decay_%        '< 1'
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.630
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.736
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.748
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.69
_refine_diff_density_min         -0.52
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.08
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         5694
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.08
_refine_ls_R_factor_all          0.021
_refine_ls_R_factor_gt           0.020
_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^)+(0.0275P)^2^+0.8849P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.051
_refine_ls_wR_factor_ref         0.051
_reflns_number_gt                5555
_reflns_number_total             5694
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ng2043.cif
_cod_data_source_block           I
_cod_original_cell_volume        1258.9(5)
_cod_database_code               2209959
_cod_database_fobs_code          2209959