A rare structural characterisation of the phosphomolybdate lacunary anion, [PMo~11~O~39~]^7-^. Crystal structures of the Ln(III) complexes, (NH~4~)~11~[Ln(PMo~11~O~39~)~2~]·16H~2~O (Ln = Ce^III^, Sm^III^, Dy^III^ or Lu^III^)
Gaunt, Andrew J.; May, Iain; Sarsfield, Mark J.; Collison, David; Helliwell, Madeleine; Denniss, Iain S.; Dalton Transactions  (2003) 2767–2771; doi:10.1039/b301995k

data_7012862
_publ_section_title
;
 A rare structural characterisation of the phosphomolybdate lacunary anion,
 [PMo~11~O~39~]^7-^. Crystal structures of the Ln(III) complexes,
 (NH~4~)~11~[Ln(PMo~11~O~39~)~2~]&#x00B7;16H~2~O (Ln = Ce^III^, Sm^III^,
 Dy^III^ or Lu^III^)
;
_journal_coden_ASTM              DTARAF
_journal_issue                   13
_journal_name_full               'Dalton Transactions'
_journal_page_first              2767
_journal_page_last               2771
_journal_paper_doi               10.1039/b301995k
_journal_year                    2003
_chemical_formula_sum            'H76 Mo22 N11 O94 P2 Sm'
_chemical_formula_weight         4057.69
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_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_date             19101-03-07
_audit_creation_method           'by teXsan v1.7'
_audit_update_record
;
?
;
_cell_angle_alpha                90.00
_cell_angle_beta                 117.77(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   38.00(3)
_cell_length_b                   13.105(10)
_cell_length_c                   19.915(10)
_cell_measurement_reflns_used    75760
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.02
_cell_measurement_theta_min      1.67
_cell_volume                     8775(11)
_computing_cell_refinement       'DENZO (Otwinowski, Z. 1988)'
_computing_data_collection       'MSC RAXIS11 Control'
_computing_data_reduction        'DENZO (Otwinowski, Z. 1988)'
_computing_publication_material  'teXsan (MSC, 1995)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
DIRDIF92 PATTY (Beurskens, 1992)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.424
_diffrn_measured_fraction_theta_max 0.424
_diffrn_measurement_device       'Rigaku RAXIS'
_diffrn_measurement_method       '80 x 3  degree phi scans'
_diffrn_radiation_detector       'image plate'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.089
_diffrn_reflns_av_sigmaI/netI    0.0835
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            75760
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.67
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.854
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.072
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             7684
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         3.258
_refine_diff_density_min         -1.810
_refine_diff_density_rms         0.274
_refine_ls_extinction_coef       0.00019(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     601
_refine_ls_number_reflns         6900
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0939
_refine_ls_R_factor_gt           0.0760
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1394P)^2^+54.1658P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2037
_refine_ls_wR_factor_ref         0.2258
_reflns_number_gt                5192
_reflns_number_total             6900
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b301995k.txt
_cod_data_source_block           s962
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1394P)^2^+54.1658P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1394P)^2^+54.1658P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        8774(11)
_cod_original_sg_symbol_H-M      'C 2/c      '
_cod_database_code               7012862