Syntheses and NLO properties of 1D heterothiometallic anionic W/S/Ag clusters possessing solvento-ytterbium cation-directed isomeric skeletons
Zhang, Jinfang; Meng, Suci; Song, Yinglin; Yang, Junyi; Wei, Hongyang; Huang, Wenjiang; Cifuentes, Marie P.; Humphrey, Mark G.; Zhang, Chi; New Journal of Chemistry 35 (2011) 328–; doi:10.1039/c0nj00674b

data_7052576
_publ_section_title
;
 Syntheses and NLO properties of 1D heterothiometallic anionic W/S/Ag
 clusters possessing solvento-ytterbium cation-directed isomeric
 skeletons
;
_journal_issue                   2
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              328
_journal_paper_doi               10.1039/c0nj00674b
_journal_volume                  35
_journal_year                    2011
_chemical_formula_iupac          '[Yb (N O3)2 (C6 H18 N3 O P)4] [W Ag S4]'
_chemical_formula_moiety         'C24 H72 N14 O10 P4 Yb +, Ag S4 W -'
_chemical_formula_sum            'C24 H72 Ag N14 O10 P4 S4 W Yb'
_chemical_formula_weight         1433.87
_chemical_name_systematic
;
catena-Poly[[tetrakis(hexamethylphosphoramide-\kO)bis(nitrato-
\k^2^O,O')ytterbium(III)]
[silver(I)-di-\m-sulfido-tungstate(VI)(Ag---W)-di-\m-sulfido]]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 90.7980(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.7241(9)
_cell_length_b                   29.5280(18)
_cell_length_c                   11.3464(7)
_cell_measurement_reflns_used    17963
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      25.3491
_cell_measurement_theta_min      3.0222
_cell_volume                     5267.6(5)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku, 2000)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2000)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku Mercury CCD (2 x 2 bin mode)'
_diffrn_measurement_method       dtprofit.ref
_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  0.0396
_diffrn_reflns_av_sigmaI/netI    0.0337
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            47611
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    4.643
_exptl_absorpt_correction_T_max  0.243
_exptl_absorpt_correction_T_min  0.097
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.808
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2836
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.932
_refine_diff_density_min         -1.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.179
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         9611
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.179
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0325
_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^)+(0.017P)^2^+19.3445P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0674
_refine_ls_wR_factor_ref         0.0686
_reflns_number_gt                9126
_reflns_number_total             9611
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            C0NJ00674B.TXT
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7052576