Insights into the Coordination Chemistry of Phosphonate Derivatives of Heteropolyoxotungstates
Richard Villanneau; David Racimor; Elisabeth Messner-Henning; Hélène Rousselière; Sébastien Picart; René Thouvenot; Anna Proust; Inorganic Chemistry 50 (2011) 1164–1166; doi:10.1021/ic102223w

data_4324479
_publ_contact_author
;
 R. Villanneau
;
_publ_contact_author_email       richard.villanneau@upmc.fr
_publ_contact_author_fax         '+33 (0) 1 44 27 38 41'
_publ_contact_author_phone       '+33 (0) 1 44 27 35 22'
_publ_section_title
;
 Insights into the Coordination Chemistry of Phosphonate Derivatives of
 Heteropolyoxotungstates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1164
_journal_page_last               1166
_journal_paper_doi               10.1021/ic102223w
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety
'La2, P2 W18 O68, 4(P1 O1 C4 H9), 10(N1 O1 C3 H7), 6(H2 O1), 4(N1 C16 H36)'
_chemical_formula_sum            'C110 H262 La2 N14 O88 P6 W18'
_chemical_formula_weight         6962.28
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.792(11)
_cell_angle_beta                 97.239(13)
_cell_angle_gamma                107.305(12)
_cell_formula_units_Z            1
_cell_length_a                   14.233(2)
_cell_length_b                   16.8840(16)
_cell_length_c                   22.433(3)
_cell_measurement_reflns_used    202
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      21
_cell_measurement_theta_min      3
_cell_volume                     5098.3(12)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (Giacovazzo, 1993)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_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  0.0607
_diffrn_reflns_av_sigmaI/netI    0.0818
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            83239
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.53
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.643
_exptl_absorpt_correction_T_max  0.0610
_exptl_absorpt_correction_T_min  0.0349
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
Interpolation using  Int.Tab. Vol. C (1992) p. 523,Tab. 6.3.3.3
for values of muR in the range 0-2.5, and Int.Tab. Vol.II (1959)
p.302; Table 5.3.6 B for muR in the range 2.6-10.0.
The interpolation procedure of C.W.Dwiggins Jr (Acta Cryst.(1975)
A31,146-148) is used with some modification.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.268
_exptl_crystal_description       prism
_exptl_crystal_F_000             3260
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.25
_refine_diff_density_max         3.331
_refine_diff_density_min         -4.008
_refine_diff_density_rms         0.376
_refine_ls_extinction_coef       0.00027(4)
_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   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     979
_refine_ls_number_reflns         29073
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0924
_refine_ls_R_factor_gt           0.0589
_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^)+(0.0832P)^2^+24.9243P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1485
_refine_ls_wR_factor_ref         0.1653
_reflns_number_gt                20584
_reflns_number_total             29073
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102223w_si_002.cif
_cod_data_source_block           (^n^Bu~4~N)~2~-2-^t^Bu-DMF
_cod_original_cell_volume        5098.4(12)
_cod_database_code               4324479