Influence of Steric and Electronic Properties of the Defect Site, Lanthanide Ionic Radii, and Solution Conditions on the Composition of Lanthanide(III) α1-P2W17O6110-Polyoxometalates
Cheng Zhang; Robertha C. Howell; Qun-Hui Luo; Heidi L. Fieselmann; Louis J. Todaro; Lynn C. Francesconi; Inorganic Chemistry 44 (2005) 3569–3578; doi:10.1021/ic050103o

data_1100737
_publ_section_title
;

Influence of Steric and Electronic Properties of the Defect Site,

Lanthanide Ionic Radii, and Solution Conditions on the Composition of

Lanthanide(III) \a1-P2W17O6110-Polyoxometalates

;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3569
_journal_page_last               3578
_journal_paper_doi               10.1021/ic050103o
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'Cl4 H92 K4 Na6 Nd O162 P4 W34'
_chemical_formula_weight         9593.92
_chemical_name_systematic
; 

 ? 

;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 104.63(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   41.072(8)
_cell_length_b                   16.152(3)
_cell_length_c                   24.933(5)
_cell_measurement_temperature    100(2)
_cell_volume                     16004(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_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  0.2791
_diffrn_reflns_av_sigmaI/netI    0.2139
_diffrn_reflns_limit_h_max       52
_diffrn_reflns_limit_h_min       -52
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            59874
_diffrn_reflns_theta_full        27.32
_diffrn_reflns_theta_max         27.32
_diffrn_reflns_theta_min         2.90
_exptl_absorpt_coefficient_mu    24.980
_exptl_absorpt_correction_T_max  0.1890
_exptl_absorpt_correction_T_min  0.0314
_exptl_absorpt_process_details
'Numerical absorption correction from indexed crystal faces'
_exptl_crystal_density_diffrn    3.982
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             16848
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.10
_refine_diff_density_max         6.177
_refine_diff_density_min         -6.372
_refine_diff_density_rms         1.162
_refine_ls_extinction_coef       0.000070(7)
_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   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     540
_refine_ls_number_reflns         17288
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.1846
_refine_ls_R_factor_gt           0.1221
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1544P)^2^+9812.2217P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2982
_refine_ls_wR_factor_ref         0.3469
_reflns_number_gt                10779
_reflns_number_total             17288
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050103osi20050113_051640.cif
_cod_data_source_block           Neodymium_a1P2W17O61_1to2
_cod_original_formula_sum        'H46 Cl2 K2 Na2 Nd0.50 O81 P2 W17'
_cod_database_code               1100737