Phase transformation of a rare-earth Anderson polyoxometalate at low temperature
Zhang, Li-Zhi; Gu, Wen; Dong, Zhili; Liu, Xin; Li, Bing; CrystEngComm 10 (2008) 1318–; doi:10.1039/b808085b

data_7202245
_publ_section_title
;
 Phase transformation of a rare-earth Anderson polyoxometalate at low
 temperature
;
_journal_issue                   10
_journal_name_full               CrystEngComm
_journal_page_first              1318
_journal_paper_doi               10.1039/b808085b
_journal_volume                  10
_journal_year                    2008
_chemical_formula_moiety         'H72 Cr2 Mo12 O78 Tm2'
_chemical_formula_sum            'Cr2 H72 Mo12 O78 Tm2'
_chemical_formula_weight         2913.72
_chemical_name_systematic
;
?
;
_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                86.667(12)
_cell_angle_beta                 72.242(9)
_cell_angle_gamma                64.394(9)
_cell_formula_units_Z            2
_cell_length_a                   15.607(4)
_cell_length_b                   15.934(5)
_cell_length_c                   16.088(5)
_cell_measurement_reflns_used    7154
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      1.5
_cell_volume                     3423.3(18)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'CrystalStructure 3.7.0'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'Rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0468
_diffrn_reflns_av_sigmaI/netI    0.0709
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            26405
_diffrn_reflns_theta_full        27.90
_diffrn_reflns_theta_max         27.90
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    5.114
_exptl_absorpt_correction_T_max  0.5346
_exptl_absorpt_correction_T_min  0.4950
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    2.827
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2772
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         4.086
_refine_diff_density_min         -3.695
_refine_diff_density_rms         0.296
_refine_ls_extinction_coef       0.00083(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   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     858
_refine_ls_number_reflns         16114
_refine_ls_number_restraints     162
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0434
_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^)+(0.0517P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1073
_refine_ls_wR_factor_ref         0.1265
_reflns_number_gt                9944
_reflns_number_total             16114
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b808085b.txt
_cod_data_source_block           1'
_cod_original_cell_volume        3423.3(17)
_cod_original_formula_sum        'H72 Cr2 Mo12 O78 Tm2'
_cod_database_code               7202245