Organic‒Inorganic Hybrids Based on Monovacant Keggin-type Silicotungstates and 3d-4f Heterometals
Zhang, Shaowei; Zhao, Junwei; Ma, Pengtao; Chen, Huanni; Niu, Jingyang; Wang, Jingping; Crystal Growth & Design 12 (2012) 1263–; doi:10.1021/cg2012759

data_4505494
_publ_section_title
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 Organic--Inorganic Hybrids Based on Monovacant Keggin-type
 Silicotungstates and 3d-4f Heterometals
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_journal_issue                   3
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              1263
_journal_paper_doi               10.1021/cg2012759
_journal_volume                  12
_journal_year                    2012
_chemical_formula_sum            'C16 H85 Cu3 N16 O85 Pr Si2 W22'
_chemical_formula_weight         6294.34
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 101.698(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.816(12)
_cell_length_b                   11.667(7)
_cell_length_c                   39.20(2)
_cell_measurement_reflns_used    9860
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.70
_cell_measurement_theta_min      2.36
_cell_volume                     9770(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 0.979
_diffrn_measured_fraction_theta_max 0.979
_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  0.0531
_diffrn_reflns_av_sigmaI/netI    0.0674
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            39705
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    27.042
_exptl_absorpt_correction_T_max  0.0700
_exptl_absorpt_correction_T_min  0.0492
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    4.273
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             11064
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_refine_diff_density_max         4.945
_refine_diff_density_min         -2.294
_refine_diff_density_rms         0.384
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1238
_refine_ls_number_reflns         16849
_refine_ls_number_restraints     281
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0455
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0393P)^2^+88.9043P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0920
_refine_ls_wR_factor_ref         0.0992
_reflns_number_gt                12748
_reflns_number_total             16849
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg2012759_si_001.cif
_cod_data_source_block           8
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' 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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        9771(10)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4505494