Chloridobis(pyrrolidine-1-dithiocarboxylato-κ^2^<i>S</i>,<i>S</i>')antimony(III)
Zhai, Jun; Yin, Handong; Li, Feng; Wang, Daqi; Acta Crystallographica Section E 63 (2007) m2871–m2871; doi:10.1107/S1600536807053962

data_2216654
_publ_section_title
Chloridobis(pyrrolidine-1-dithiocarboxylato-\k^2^<i>S</i>,<i>S</i>')antimony(III)
_journal_coeditor_code           LX2025
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2871
_journal_page_last               m2871
_journal_paper_doi               10.1107/S1600536807053962
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Sb (C5 H8 N S2)2 Cl]'
_chemical_formula_moiety         'C10 H16 Cl1 N2 S4 Sb'
_chemical_formula_sum            'C10 H16 Cl N2 S4 Sb'
_chemical_formula_weight         449.69
_chemical_melting_point          421
_chemical_name_systematic
;
Chloridobis(pyrrolidine-1-dithiocarboxylato-
\k^2^<i>S</i>,<i>S</i>')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                111.451(3)
_cell_angle_beta                 91.950(3)
_cell_angle_gamma                102.334(3)
_cell_formula_units_Z            2
_cell_length_a                   6.367(2)
_cell_length_b                   10.368(3)
_cell_length_c                   13.414(4)
_cell_measurement_reflns_used    2270
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.182
_cell_measurement_theta_min      2.176
_cell_volume                     799.0(4)
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        'Please supply'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997b)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w 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  0.0157
_diffrn_reflns_av_sigmaI/netI    0.0323
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4147
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.64
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.401
_exptl_absorpt_correction_T_max  0.748
_exptl_absorpt_correction_T_min  0.540
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.869
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             444
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.496
_refine_diff_density_min         -0.389
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         2764
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0267
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0198P)^2^+0.5878P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0539
_refine_ls_wR_factor_ref         0.0602
_reflns_number_gt                2300
_reflns_number_total             2764
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lx2025.cif
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     -p_1
_cod_database_code               2216654
_cod_database_fobs_code          2216654