Heterometallic Polymeric Clusters Containing Tetraselenotungstate Anion: One-Dimensional Helical Chain {[La(Me2SO)8][(μ-WSe4)3Ag3]}n and Cyanide-Bridged Three-Dimensional Cross-Framework {[Et4N]2[(μ4-WSe4)Cu4(CN)4]}n
Qian-Feng Zhang; Wa-Hung Leung; Xin; Hoong-Kun Fun; Inorganic Chemistry 39 (2000) 417–426; doi:10.1021/ic990780g

data_4300085
_publ_section_title
;
Heterometallic Polymeric Clusters Containing Tetraselenotungstate Anion:
One-Dimensional Helical Chain {[La(Me2SO)8][(\m-WSe4)3Ag3]}n and
Cyanide-Bridged Three-Dimensional Cross-Framework
{[Et4N]2[(\m4-WSe4)Cu4(CN)4]}n
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              417
_journal_page_last               426
_journal_paper_doi               10.1021/ic990780g
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C16 H48 Ag3 La O8 S8 Se12 W3'
_chemical_formula_weight         2586.61
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 103.564(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.7642(5)
_cell_length_b                   24.1725(9)
_cell_length_c                   19.4012(7)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.38
_cell_measurement_theta_min      1.37
_cell_volume                     5819.1(4)
_computing_cell_refinement       'SAINT (Siemens, 1996b)'
_computing_data_collection       'SMART (Siemens, 1996a)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material
;
SHELXTL, PARST (Nardelli, 1995) and PLATON (Spek, 1990)
;
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type
;
Siemens SMART CCD area detector diffractometer
;
_diffrn_measurement_method       '\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  0.0911
_diffrn_reflns_av_sigmaI/netI    0.1098
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            39577
_diffrn_reflns_theta_full        28.39
_diffrn_reflns_theta_max         28.39
_diffrn_reflns_theta_min         1.37
_exptl_absorpt_coefficient_mu    15.434
_exptl_absorpt_correction_T_max  0.1915
_exptl_absorpt_correction_T_min  0.0505
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.952
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4656
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.708
_refine_diff_density_min         -2.018
_refine_diff_density_rms         0.261
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.945
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     494
_refine_ls_number_reflns         14315
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.945
_refine_ls_R_factor_all          0.1251
_refine_ls_R_factor_gt           0.0540
_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^)+(0.0488P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1116
_refine_ls_wR_factor_ref         0.1360
_reflns_number_gt                7593
_reflns_number_total             14315
_reflns_threshold_expression     'I > 2\s(I)'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4300085