Encapsulation of polyoxometalates within layered metal‒organic frameworks with topological and pore control
He, Zhi; Pang, Qingqing; Rankine, Damien; Sumby, Christopher J.; Zhang, Lijuan; Doonan, Christian J.; Li, Qiaowei; CrystEngComm 15 (2013) 9340–; doi:10.1039/c3ce41136b

data_7211035
_publ_section_title
;
 Encapsulation of polyoxometalates within layered metal--organic
 frameworks with topological and pore control
;
_journal_issue                   45
_journal_name_full               CrystEngComm
_journal_page_first              9340
_journal_paper_doi               10.1039/c3ce41136b
_journal_volume                  15
_journal_year                    2013
_chemical_formula_sum            'C48 H36 Cu6 O70 P W12'
_chemical_formula_weight         4351.18
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           147
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            1
_cell_length_a                   18.7659(11)
_cell_length_b                   18.7659(11)
_cell_length_c                   11.3114(13)
_cell_measurement_reflns_used    1284
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      21.05
_cell_measurement_theta_min      1.99
_cell_volume                     3449.7(5)
_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 0.980
_diffrn_measured_fraction_theta_max 0.980
_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  0.0639
_diffrn_reflns_av_sigmaI/netI    0.0599
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            28318
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    10.944
_exptl_absorpt_correction_T_max  0.2616
_exptl_absorpt_correction_T_min  0.1415
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.094
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1961
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
Very little remaining electron density was left, 
because of the highly disordered nature of solvent 
molecules.SQUEEZE shows about 180 electron counts in 
voids in each unit cell, which accounts for about 4.5
DMF molecules.
;
_refine_diff_density_max         6.603
_refine_diff_density_min         -3.999
_refine_diff_density_rms         0.466
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.187
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         5213
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.186
_refine_ls_R_factor_all          0.1406
_refine_ls_R_factor_gt           0.1045
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3207
_refine_ls_wR_factor_ref         0.3418
_reflns_number_gt                2978
_reflns_number_total             5213
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce41136b.txt
_cod_data_source_block           platon
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P-3
_cod_database_code               7211035