Polyoxomolybdates Functionalized with Phosphonocarboxylates
Ulrich Kortz; Catherine Marquer; René Thouvenot; Martine Nierlich; Inorganic Chemistry 42 (2003) 1158–1162; doi:10.1021/ic026140m

data_4313194
_publ_contact_author_address
; 
International University Bremen
School of Engineering and Science
Campus Ring 1
28759 Bremen
Germany
;
_publ_contact_author_email
;
u.kortz@iu-bremen.de
;
_publ_contact_author_fax
;
+49-421-200 3103
;
_publ_contact_author_name
;
Ulrich KORTZ
;
_publ_contact_author_phone
;
+49-421-200 3235
;
_publ_section_title
;
 Polyoxomolybdates Functionalized with Phosphonocarboxylates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1158
_journal_page_last               1162
_journal_paper_doi               10.1021/ic026140m
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C4 H6 K Mo5 O26 P2 Rb4'
_chemical_formula_weight         1415.75
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           'manual editing of SHELXL-97 file'
_cell_angle_alpha                90.00
_cell_angle_beta                 94.88(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.146(2)
_cell_length_b                   13.704(3)
_cell_length_c                   20.577(4)
_cell_measurement_reflns_used    17828
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     2850.7(10)
_computing_cell_refinement       'DENZO(Otwinowski& Minor,1997)'
_computing_data_collection       'DENZO(Otwinowski& Minor,1997)'
_computing_data_reduction        'DENZO(Otwinowski& Minor,1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick,1997)'
_computing_publication_material  'SHELXTL (Sheldrick,1997)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1990)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Nonius Kappa CCD diffractometer'
_diffrn_measurement_method       '\f rotation scans with 1\%steps'
_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  0.0573
_diffrn_reflns_av_sigmaI/netI    0.0471
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            17343
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         2.48
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    9.284
_exptl_absorpt_correction_T_max  0.543
_exptl_absorpt_correction_T_min  0.453
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'MULABS in PLATON;Spek,1998'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.240
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2572
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         4.425
_refine_diff_density_min         -3.297
_refine_diff_density_rms         0.280
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         4783
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0543
_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^)+(0.0712P)^2^+62.0912P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1376
_refine_ls_wR_factor_ref         0.1449
_reflns_number_gt                4095
_reflns_number_total             4783
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic026140m_s1.cif
_cod_data_source_block           174abstest
_cod_database_code               4313194