Construction and property investigation of inorganic-organic hybrid materials based on metal-salens and Keggin polyoxometalates
Xing Meng; Hai-Ning Wang; Xin-Long Wang; Guang-Sheng Yang; Shuang Wang; Kui-Zhan Shao; Zhong-Min Su; Inorganica Chimica Acta 390 (2012) 135–142; doi:10.1016/j.ica.2012.04.011

data_1512402
_publ_section_title
;
 Construction and property investigation of inorganic-organic hybrid
 materials based on metal-salens and Keggin polyoxometalates
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              135
_journal_page_last               142
_journal_paper_doi               10.1016/j.ica.2012.04.011
_journal_volume                  390
_journal_year                    2012
_chemical_formula_moiety         'C64 H60 Cu6 N8 O50 Si W12'
_chemical_formula_sum            'C64 H60 Cu6 N8 O50 Si W12'
_chemical_formula_weight         4356.73
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   14.939(5)
_cell_length_b                   23.406(5)
_cell_length_c                   34.243(5)
_cell_measurement_reflns_used    58870
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.31
_cell_measurement_theta_min      1.19
_cell_volume                     11973(5)
_computing_cell_refinement       'SMART (Bruker, 1997)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL-PLUS (Sheldrick, 1990)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97(Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1242
_diffrn_reflns_av_sigmaI/netI    0.1042
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            58870
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.31
_diffrn_reflns_theta_min         1.19
_exptl_absorpt_coefficient_mu    12.599
_exptl_absorpt_correction_T_max  0.061
_exptl_absorpt_correction_T_min  0.055
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS(Sheldrick, 1996)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.417
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7904
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_platon_squeeze_details          ' ?'
_refine_diff_density_max         2.481
_refine_diff_density_min         -4.088
_refine_diff_density_rms         0.293
_refine_ls_extinction_coef       0.000015(7)
_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   0.960
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     614
_refine_ls_number_reflns         10859
_refine_ls_number_restraints     410
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1190
_refine_ls_R_factor_gt           0.0692
_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^)+(0.1127P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1853
_refine_ls_wR_factor_ref         0.2084
_reflns_number_gt                5758
_reflns_number_total             10859
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2012-390-135-142-4.cif
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'Pbca '
_cod_database_code               1512402