New Polyoxometalate Compounds Built up of Lacunary Wells‒Dawson Anions and Trivalent Lanthanide Cations
Lu, Ying; Xu, Yan; Li, Yangguang; Wang, Enbo; Xu, Xinxin; Ma, Ying; Inorganic Chemistry 45 (2006) 2055–2060; doi:10.1021/ic0515857

data_1101172
_publ_section_title
;
 New Polyoxometalate Compounds Built up of Lacunary Wells--Dawson Anions
 and Trivalent Lanthanide Cations
;
_journal_coden_ASTM              INOCAJ
_journal_issue                   5
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2055
_journal_page_last               2060
_journal_paper_doi               10.1021/ic0515857
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C20 H47 N4 Nd2 O74.5 P2 W17'
_chemical_formula_weight         5011.49
_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                88.24(3)
_cell_angle_beta                 76.11(3)
_cell_angle_gamma                64.66(3)
_cell_formula_units_Z            2
_cell_length_a                   12.904(3)
_cell_length_b                   12.951(3)
_cell_length_c                   25.514(5)
_cell_measurement_temperature    293(2)
_cell_volume                     3728.4(13)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_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      293(2)
_diffrn_detector_area_resol_mean 0.01
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID IP'
_diffrn_measurement_method       Oscillation
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rotation anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0632
_diffrn_reflns_av_sigmaI/netI    0.0825
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            29529
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.01
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    27.636
_exptl_absorpt_correction_T_max  0.0410
_exptl_absorpt_correction_T_min  0.0338
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR by T.Higashi    8 March, 1995'
_exptl_crystal_colour            'pale pink'
_exptl_crystal_density_diffrn    4.464
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4398
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.32
_refine_diff_density_max         2.321
_refine_diff_density_min         -3.055
_refine_diff_density_rms         0.461
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1090
_refine_ls_number_reflns         13080
_refine_ls_number_restraints     780
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0457
_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^)+(0.0118P)^2^+81.8297P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0892
_refine_ls_wR_factor_ref         0.0950
_reflns_number_gt                10528
_reflns_number_total             13080
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0515857si20060104_092410.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_formula_sum        'C20 H47 N4 Nd2 O74.50 P2 W17'
_cod_database_code               1101172