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_4305259
_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            'H71 Hf Mo23 N6 O102.5 P2'
_chemical_formula_weight         4242.68
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 114.223(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.3813(6)
_cell_length_b                   37.9050(11)
_cell_length_c                   20.5948(8)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.2377
_cell_measurement_theta_min      4.78
_cell_volume                     9526.3(7)
_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_detector_area_resol_mean 8.3367
_diffrn_measured_fraction_theta_full 0.884
_diffrn_measured_fraction_theta_max 0.884
_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  0.0395
_diffrn_reflns_av_sigmaI/netI    0.0539
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            47173
_diffrn_reflns_theta_full        26.29
_diffrn_reflns_theta_max         26.29
_diffrn_reflns_theta_min         4.79
_exptl_absorpt_coefficient_mu    4.142
_exptl_absorpt_correction_T_max  0.59487
_exptl_absorpt_correction_T_min  0.22998
_exptl_absorpt_correction_type   'numerical analytical'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.958
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             8004
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.085
_refine_diff_density_min         -4.262
_refine_diff_density_rms         0.324
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1128
_refine_ls_number_reflns         17086
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0689
_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^)+(0.0552P)^2^+493.6367P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1700
_refine_ls_wR_factor_ref         0.1784
_reflns_number_gt                13351
_reflns_number_total             17086
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800101t-file002_3.cif
_cod_data_source_block           oim17pn
_cod_original_cell_volume        9526.3(6)
_cod_original_formula_sum        'H71 Hf Mo23 N6 O102.50 P2'
_cod_database_code               4305259