Tetravalent Metal Complexation by Keggin and Lacunary Phosphomolybdate Anions
Roy Copping; Leif Jonasson; Andrew J. Gaunt; Dennis Drennan; David Collison; Madeleine Helliwell; Ross J. Pirttijarvi; Chris J. Jones; Anne Huguet; David C. Apperley; Nikolas Kaltsoyannis; Iain May; Inorganic Chemistry 47 (2008) 5787–5798; doi:10.1021/ic800101t

data_4305257
_publ_contact_author
;
    Roy Copping
;
_publ_section_title
;
Tetravalent Metal Complexation by Keggin and Lacunary Phosphomolybdate
Anions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5787
_journal_page_last               5798
_journal_paper_doi               10.1021/ic800101t
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'Ce Cs10 H40 Mo22 O98 P2'
_chemical_formula_weight         5250.16
_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_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 118.149(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   37.7066(15)
_cell_length_b                   13.3093(5)
_cell_length_c                   19.9971(7)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.9311
_cell_measurement_theta_min      2.65
_cell_volume                     8848.6(8)
_computing_cell_refinement
;

CrysAlis RED, Oxford Diffraction Ltd.,

Version 1.171.28cycle4 beta (release 11-11-2005 CrysAlis171 .NET)

(compiled Nov 11 2005,15:50:43)

;
_computing_data_collection
;

CrysAlis CCD, Oxford Diffraction Ltd.,

Version 1.171.28cycle4 beta (release 11-11-2005 CrysAlis171 .NET)

(compiled Nov 11 2005,15:50:43)

;
_computing_data_reduction
;

CrysAlis RED, Oxford Diffraction Ltd.,

Version 1.171.28cycle4 beta (release 11-11-2005 CrysAlis171 .NET)

(compiled Nov 11 2005,15:50:43)

;
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.931
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_device_type  'Oxford Diffraction XCalibur 2'
_diffrn_measurement_method       'phi and omega'
_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  0.0378
_diffrn_reflns_av_sigmaI/netI    0.0447
_diffrn_reflns_limit_h_max       54
_diffrn_reflns_limit_h_min       -55
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            45889
_diffrn_reflns_theta_full        32.00
_diffrn_reflns_theta_max         32.00
_diffrn_reflns_theta_min         3.06
_exptl_absorpt_coefficient_mu    7.727
_exptl_absorpt_correction_T_max  0.64
_exptl_absorpt_correction_T_min  0.38
_exptl_absorpt_correction_type   'numeric analytical'
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.941
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             9544
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         10.323
_refine_diff_density_min         -3.648
_refine_diff_density_rms         0.325
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_matrix_type           full
_refine_ls_number_parameters     582
_refine_ls_number_reflns         14305
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0425
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0511P)^2^+56.7378P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0974
_refine_ls_wR_factor_ref         0.1036
_reflns_number_gt                11633
_reflns_number_total             14305
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800101t-file002_1.cif
_cod_data_source_block           oim36sadabsc
_cod_original_cell_volume        8848.5(6)
_cod_original_formula_sum        'H40 Ce Cs10 Mo22 O98 P2'
_cod_database_code               4305257