Novel Rare Earth Germanotungstates and Organic Hybrid Derivatives: Synthesis and Structures of M/[α-GeW11O39] (M = Nd, Sm, Y, Yb) and Sm/[α-GeW11O39](DMSO)
Wang, Jing-Ping; Duan, Xian-Ying; Du, Xiao-Di; Niu, Jing-Yang; Crystal Growth & Design 6 (2006) 2266–; doi:10.1021/cg050321s

data_4508618
_publ_section_title
;
 Novel Rare Earth Germanotungstates and Organic Hybrid
 Derivatives:&#x2009; Synthesis and Structures of M/[\a-GeW11O39] (M = Nd,
 Sm, Y, Yb) and Sm/[\a-GeW11O39](DMSO)
;
_journal_issue                   10
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              2266
_journal_paper_doi               10.1021/cg050321s
_journal_volume                  6
_journal_year                    2006
_chemical_formula_sum            'C8 H43.5 Ge N2 Nd1.5 O48 W11'
_chemical_formula_weight         3247.25
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_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                 105.75(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.846(4)
_cell_length_b                   13.443(3)
_cell_length_c                   27.561(6)
_cell_measurement_temperature    293(2)
_cell_volume                     6720(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.934
_diffrn_measured_fraction_theta_max 0.934
_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  0.0419
_diffrn_reflns_av_sigmaI/netI    0.0575
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            19527
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    20.401
_exptl_absorpt_correction_T_max  0.1933
_exptl_absorpt_correction_T_min  0.1126
_exptl_crystal_density_diffrn    3.210
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5702
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.448
_refine_diff_density_min         -2.168
_refine_diff_density_rms         0.427
_refine_ls_extinction_coef       0.000230(17)
_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   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     722
_refine_ls_number_reflns         11053
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0546
_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^)+(0.0909P)^2^+10.5544P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1368
_refine_ls_wR_factor_ref         0.1445
_reflns_number_gt                9455
_reflns_number_total             11053
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg050321ssup1.cif
_cod_data_source_block           njy1
_cod_original_cell_volume        6720(2)
_cod_original_formula_sum        'C8 H43.50 Ge N2 Nd1.50 O48 W11'
_cod_database_code               4508618