The First Example of Solvothermally Synthesized Thioantimonates(V) with Ethylenediamine Coordinated Lanthanide(III): [Sm(en)4]SbS4.0.5en and [Sm(en)3(H2O)(μ-SbS4)]\ιnfty
Ding-xian Jia; Qin-Yu Zhu; Jie Dai; Wen Lu; Wen-Juan Guo; Inorganic Chemistry 44 (2005) 819–821; doi:10.1021/ic0484957

data_4308539
_publ_section_title
;
The First Example of Solvothermally Synthesized Thioantimonates(V) with
Ethylenediamine Coordinated Lanthanide(III): [Sm(en)4]SbS4.0.5en and
[Sm(en)3(H2O)(\m-SbS4)]\\infty
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              819
_journal_page_last               821
_journal_paper_doi               10.1021/ic0484957
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'C6 H26 N6 O S4 Sb Sm'
_chemical_formula_sum            'C6 H26 N6 O S4 Sb Sm'
_chemical_formula_weight         598.67
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      62
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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            4
_cell_length_a                   9.2725(6)
_cell_length_b                   13.3851(9)
_cell_length_c                   14.6863(9)
_cell_measurement_reflns_used    7623
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     1822.8(2)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Rigaku Mercury'
_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  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0188
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19104
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    5.131
_exptl_absorpt_correction_T_max  0.5132
_exptl_absorpt_correction_T_min  0.2905
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            light-Yellow
_exptl_crystal_density_diffrn    2.182
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1156
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.017
_refine_diff_density_min         -0.820
_refine_diff_density_rms         0.116
_refine_ls_extinction_coef       0.00278(10)
_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   1.149
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     94
_refine_ls_number_reflns         2162
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.0221
_refine_ls_R_factor_gt           0.0214
_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^)+(0.0142P)^2^+5.7694P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0499
_refine_ls_wR_factor_ref         0.0503
_reflns_number_gt                2121
_reflns_number_total             2162
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0484957si20041213_092950.cif
_cod_data_source_block           shelxl
_cod_original_sg_symbol_Hall     '-p 2ac 2n'
_cod_database_code               4308539