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_4324481
_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
'Zr2, P2 W18 O68, 4(P1 O1 C4 H9), 6(N1 O1 C3 H7), 2(H1 O1), 4(N1 C16 H36)'
_chemical_formula_sum            'C98 H224 N10 O80 P6 W18 Zr2'
_chemical_formula_weight         6500.43
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_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                 93.381(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.162(4)
_cell_length_b                   27.858(5)
_cell_length_c                   20.453(3)
_cell_measurement_reflns_used    361
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24
_cell_measurement_theta_min      3
_cell_volume                     8624(3)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0656
_diffrn_reflns_av_sigmaI/netI    0.0711
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            89997
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.58
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.204
_exptl_absorpt_correction_T_max  0.295
_exptl_absorpt_correction_T_min  0.0531
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.503
_exptl_crystal_description       stick
_exptl_crystal_F_000             6048
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.086
_refine_diff_density_min         -2.486
_refine_diff_density_rms         0.267
_refine_ls_extinction_coef       0.000120(9)
_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   0.980
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1022
_refine_ls_number_reflns         25028
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.0722
_refine_ls_R_factor_gt           0.0379
_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^)+(0.0390P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0738
_refine_ls_wR_factor_ref         0.0832
_reflns_number_gt                17742
_reflns_number_total             25028
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102223w_si_004.cif
_cod_data_source_block           (^n^Bu~4~N)~4~-1-^t^Bu-DMF
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4324481