Production and reactions of organic-soluble lanthanide complexes of the monolacunary Dawson [alpha1-P2W17O61]10- polyoxotungstate.
Boglio, Cécile; Lenoble, Géraldine; Duhayon, Carine; Hasenknopf, Bernold; Thouvenot, René; Zhang, Cheng; Howell, Robertha C.; Burton-Pye, Benjamin P; Francesconi, Lynn C.; Lacôte, Emmanuel; Thorimbert, Serge; Malacria, Max; Afonso, Carlos; Tabet, Jean-Claude; Inorganic chemistry 45 (2006) 1389–1398; doi:10.1021/ic051679g

data_4340198
_publ_section_title
;
 Production and reactions of organic-soluble lanthanide complexes of the
 monolacunary Dawson [alpha1-P2W17O61]10- polyoxotungstate.
;
_journal_issue                   3
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1389
_journal_page_last               1398
_journal_paper_doi               10.1021/ic051679g
_journal_volume                  45
_journal_year                    2006
_chemical_compound_source
;
?
;
_chemical_formula_moiety         ' 14(K+), (H16 La2 O130 P4 W34)14-, 14(H2O) '
_chemical_formula_sum            'H44 K14 La2 O144 P4 W34'
_chemical_formula_weight         9548.24
_chemical_name_systematic
;                                                                               
?                                                                               
;
_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
_audit_creation_date             03-20-02
_audit_creation_method           CRYSTALS_ver_12-03-99
_cell_angle_alpha                90.0
_cell_angle_beta                 92.857(17)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.008(2)
_cell_length_b                   21.225(4)
_cell_length_c                   28.835(6)
_cell_measurement_reflns_used    137
_cell_measurement_temperature    295
_cell_measurement_theta_max      20.3
_cell_measurement_theta_min      4.3
_cell_volume                     7951(3)
_computing_cell_refinement
; 
 Denzo/Scalepack (Otwinowski & Minor, 1996) 
;
_computing_data_collection
; 
 COLLECT (Nonius BV, 1997) 
;
_computing_data_reduction
; 
 Denzo/Scalepack (Otwinowski & Minor, 1996) 
;
_computing_molecular_graphics
; 
 CAMERON (Watkin et al 1996) 
;
_computing_publication_material
; 
 CRYSTALS (Watkin et al 2001) 
;
_computing_structure_refinement
; 
 CRYSTALS (Watkin et al 2001) 
;
_computing_structure_solution
; 
 USER DEFINED STRUCTURE SOLUTION 
;
_diffrn_ambient_temperature      295
_diffrn_measured_fraction_theta_full 0.949
_diffrn_measured_fraction_theta_max 0.828
_diffrn_measurement_device_type
; 
Enraf Nonius Kappa CCD 
;
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.29
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            39353
_diffrn_reflns_theta_full        22.590
_diffrn_reflns_theta_max         30.020
_diffrn_reflns_theta_min         1.192
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    25.51
_exptl_absorpt_correction_T_max  0.08
_exptl_absorpt_correction_T_min  0.07
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
; 
 DIFABS (Walker & Stuart, 1983) 
;
_exptl_crystal_colour            ' colorless '
_exptl_crystal_density_diffrn    3.99
_exptl_crystal_description       ' parallelepiped '
_exptl_crystal_F_000             8304.00
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_refine_diff_density_max         3.81
_refine_diff_density_min         -4.17
_refine_ls_extinction_coef       72.6
_refine_ls_extinction_method
'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_ref   1.1026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     476
_refine_ls_number_reflns         7424
_refine_ls_R_factor_all          0.1721
_refine_ls_R_factor_gt           0.0705
_refine_ls_shift/su_max          0.002158
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method = Prince modified Chebychev polynomial, (Watkin, 1994) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2]^2 

 
 0.677 0.480 0.367 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1637
_refine_ls_wR_factor_gt          0.0780
_refine_ls_wR_factor_ref         0.0779
_reflns_limit_h_max              18
_reflns_limit_h_min              -18
_reflns_limit_k_max              29
_reflns_limit_k_min              0
_reflns_limit_l_max              40
_reflns_limit_l_min              0
_reflns_number_gt                7437
_reflns_number_total             19212
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            ic051679gsi20050929_120506.cif
_cod_data_source_block           CRYSTALS_cif
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        ' H44 K14 La2 O144 P4 W34 '
_cod_database_code               4340198