Polyoxometalate-Diphosphate Complexes. 6.1Possible Intermediates in the Molybdate-Catalyzed Hydrolysis of Pyrophosphate: Structure of Hexamolybdopyrophosphate [(O3POPO3)Mo6O18(H2O)4]4-
Ulrich Kortz; Inorganic Chemistry 39 (2000) 625–626; doi:10.1021/ic990959r

data_4300149
_publ_contact_author_address
;
Department of Chemistry
American University of Beirut
Bliss street, POB 11-0236
Beirut, LEBANON
;
_publ_contact_author_email
;
ulrich.kortz@aub.edu.lb
;
_publ_contact_author_fax
;
+961 1 74 44 61
;
_publ_contact_author_name
;
Kortz Ulrich
;
_publ_contact_author_phone
;
+961 3 77 64 39
;
_publ_section_title
;
Polyoxometalate-Diphosphate Complexes. 6.1Possible Intermediates in the
Molybdate-Catalyzed Hydrolysis of Pyrophosphate: Structure of
Hexamolybdopyrophosphate [(O3POPO3)Mo6O18(H2O)4]4-
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              625
_journal_page_last               626
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C36 Mo6 N4 O33 P2'
_chemical_formula_weight         1653.98
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                72.02
_cell_angle_beta                 74.19
_cell_angle_gamma                83.8310(10)
_cell_formula_units_Z            2
_cell_length_a                   12.8718(2)
_cell_length_b                   15.43660(10)
_cell_length_c                   16.1842(2)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.19
_cell_measurement_theta_min      1.37
_cell_volume                     2942.04(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.938
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_sigmaI/netI    0.0487
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            32051
_diffrn_reflns_theta_full        28.19
_diffrn_reflns_theta_max         28.19
_diffrn_reflns_theta_min         1.37
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.386
_exptl_absorpt_correction_T_max  0.772999
_exptl_absorpt_correction_T_min  0.658225
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick)'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.867
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1580
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.381
_refine_diff_density_min         -2.183
_refine_diff_density_rms         0.282
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         13568
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0918
_refine_ls_R_factor_gt           0.0696
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1292P)^2^+9.6838P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1840
_refine_ls_wR_factor_ref         0.2108
_reflns_number_gt                10148
_reflns_number_total             13568
_reflns_threshold_expression     >2sigma(I)
_cod_original_cell_volume        2942.10(6)
_cod_database_code               4300149
_journal_paper_doi 10.1021/ic990959r