A Reduced Polyoxomolybdenum Borophosphate Anion Related to the Wells-Dawson Clusters
Eddy Dumas; Catherine Debiemme-Chouvy; Slavi C. Sevov; Journal of the American Chemical Society 124 (2002) 908–909; doi:10.1021/ja012352r

data_4114607
_publ_section_title
;
 A Reduced Polyoxomolybdenum Borophosphate Anion Related to the
 Wells-Dawson Clusters
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              908
_journal_page_last               909
_journal_paper_doi               10.1021/ja012352r
_journal_volume                  124
_journal_year                    2002
_chemical_formula_moiety         (C3N2H5)8[Mo12O22(BO4)2(PO4)5(HPO4)3]4H2O
_chemical_formula_sum            'C12 H27 B Mo6 N8 O33 P4'
_chemical_formula_weight         1521.75
_chemical_name_common            'molybdenum borophosphate'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 105.060(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.060(5)
_cell_length_b                   15.001(2)
_cell_length_c                   21.9786(19)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13
_cell_measurement_theta_min      11
_cell_volume                     7979(2)
_computing_cell_refinement       CAD4_(Enraf-Nonius,_1977)
_computing_data_collection       CAD4_(Enraf-Nonius,_1977)
_computing_data_reduction        SDS_Package_(Enraf-Nonius,_1985)
_computing_molecular_graphics    'SHELXTL (Siemens, 1994)'
_computing_publication_material  'SHELXTL (Siemens, 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  Enraf_Nonius_CAD4
_diffrn_measurement_method       omega-2theta
_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  0.0605
_diffrn_reflns_av_sigmaI/netI    0.0291
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            7192
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.20
_diffrn_standards_decay_%        28.6
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.109
_exptl_absorpt_correction_T_max  0.41462
_exptl_absorpt_correction_T_min  0.32433
_exptl_absorpt_correction_type   semiempirical
_exptl_absorpt_process_details   'average of 4 psi-scans'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.534
_exptl_crystal_description       polyhedral
_exptl_crystal_F_000             5888
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.786
_refine_diff_density_min         -1.009
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     472
_refine_ls_number_reflns         7021
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0490
_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^)+(0.0769P)^2^+113.1740P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1339
_refine_ls_wR_factor_ref         0.1441
_reflns_number_gt                5767
_reflns_number_total             7021
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja012352r.cif
_cod_data_source_block           end
_cod_original_cell_volume        7978(2)
_cod_database_code               4114607