Flux Synthesis of the Noncentrosymmetric Cluster Compounds Cs2SnAs2Q9 (Q = S, Se) Containing Two Different Polychalcoarsenite β-[AsQ4]3- and [AsQ5]3- Ligands
Ratnasabapathy G. Iyer; Junghwan Do; Mercouri G. Kanatzidis; Inorganic Chemistry 42 (2003) 1475–1482; doi:10.1021/ic0260771

data_4313308
_publ_section_title
;
 Flux Synthesis of the Noncentrosymmetric Cluster Compounds Cs2SnAs2Q9 (Q
 = S, Se) Containing Two Different Polychalcoarsenite \b-[AsQ4]3- and
 [AsQ5]3- Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1475
_journal_page_last               1482
_journal_paper_doi               10.1021/ic0260771
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'As2 Cs2 Se9 Sn'
_chemical_formula_weight         1244.99
_chemical_name_systematic        Cs2SnAs2Se9
_space_group_IT_number           4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_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                 115.857(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.175(5)
_cell_length_b                   17.555(12)
_cell_length_c                   7.663(5)
_cell_measurement_temperature    296(2)
_cell_volume                     868.6(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.917
_diffrn_measured_fraction_theta_max 0.917
_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  0.1449
_diffrn_reflns_av_sigmaI/netI    0.3379
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            6787
_diffrn_reflns_theta_full        28.50
_diffrn_reflns_theta_max         28.50
_diffrn_reflns_theta_min         2.32
_exptl_absorpt_coefficient_mu    28.208
_exptl_absorpt_correction_T_max  0.6023
_exptl_absorpt_correction_T_min  0.1011
_exptl_crystal_density_diffrn    4.761
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.836
_refine_diff_density_min         -1.552
_refine_diff_density_rms         0.368
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.17(7)
_refine_ls_extinction_coef       0.0016(3)
_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   0.802
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     129
_refine_ls_number_reflns         3670
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.802
_refine_ls_R_factor_all          0.2744
_refine_ls_R_factor_gt           0.0848
_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^)+(0.0746P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1594
_refine_ls_wR_factor_ref         0.2332
_reflns_number_gt                941
_reflns_number_total             3670
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0260771_s1_2.cif
_cod_data_source_block           las2
_cod_original_cell_volume        868.5(11)
_cod_database_code               4313308