Syntheses, structures and properties of dimeric rare earth derivatives based on monovacant Keggin-type polyoxotungstates
Zhang, Dongdi; Zhang, Chao; Chen, Huanni; Ma, Pengtao; Wang, Jingping; Niu, Jingyang; Inorganica Chimica Acta 391 (2012) 218–223; doi:10.1016/j.ica.2012.04.030

data_1508158
_publ_section_title
;
 Syntheses, structures and properties of dimeric rare earth derivatives
 based on monovacant Keggin-type polyoxotungstates
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              218
_journal_page_last               223
_journal_paper_doi               10.1016/j.ica.2012.04.030
_journal_volume                  391
_journal_year                    2012
_chemical_formula_sum            'C44 H146 N10 O92 P2 W22 Y2'
_chemical_formula_weight         6572.17
_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_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 115.1560(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   25.030(2)
_cell_length_b                   12.7022(10)
_cell_length_c                   22.3103(18)
_cell_measurement_reflns_used    8158
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.36
_cell_measurement_theta_min      2.30
_cell_volume                     6420.5(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0536
_diffrn_reflns_av_sigmaI/netI    0.0659
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            31844
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         0.90
_exptl_absorpt_coefficient_mu    20.634
_exptl_absorpt_correction_T_max  0.2582
_exptl_absorpt_correction_T_min  0.1187
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.399
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             5904
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.828
_refine_diff_density_min         -3.003
_refine_diff_density_rms         0.382
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     722
_refine_ls_number_reflns         11311
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0414
_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^)+(0.0550P)^2^+2.5979P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0978
_refine_ls_wR_factor_ref         0.1091
_reflns_number_gt                8133
_reflns_number_total             11311
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            2.cif
_cod_data_source_block           njy1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to the built-in table from CIF Core dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        6420.6(9)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1508158