Mono-substituted Keggin, Wells-Dawson and {P2W21}-type polyoxometalates without positional disorder
Cao, Rui; O'Halloran, Kevin P.; Hillesheim, Daniel A.; Hardcastle, Kenneth I.; Hill, Craig L.; CrystEngComm 12 (2010) 1518–; doi:10.1039/b919934a

data_7212119
_publ_section_title
;
 Mono-substituted Keggin, Wells-Dawson and {P2W21}-type polyoxometalates
 without positional disorder
;
_journal_issue                   5
_journal_name_full               CrystEngComm
_journal_page_first              1518
_journal_paper_doi               10.1039/b919934a
_journal_volume                  12
_journal_year                    2010
_chemical_formula_moiety         'C16 H45 K N5 O78 P2 Rb0 Sn W20'
_chemical_formula_sum            'C16 H45 K N5 O78 P2 Rb0 Sn W20'
_chemical_formula_weight         5452.30
_chemical_name_systematic
;
?
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.789(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.0559(17)
_cell_length_b                   40.252(5)
_cell_length_c                   17.858(3)
_cell_measurement_reflns_used    9234
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.11
_cell_measurement_theta_min      2.28
_cell_volume                     8885(2)
_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      173(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_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  0.0884
_diffrn_reflns_av_sigmaI/netI    0.0620
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       57
_diffrn_reflns_limit_k_min       -55
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            168521
_diffrn_reflns_theta_full        30.42
_diffrn_reflns_theta_max         30.42
_diffrn_reflns_theta_min         1.01
_exptl_absorpt_coefficient_mu    26.239
_exptl_absorpt_correction_T_max  0.2011
_exptl_absorpt_correction_T_min  0.1021
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    4.076
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             9516
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_refine_diff_density_max         7.044
_refine_diff_density_min         -4.450
_refine_diff_density_rms         0.561
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     633
_refine_ls_number_reflns         26062
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0765
_refine_ls_R_factor_gt           0.0557
_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^)+(0.0320P)^2^+580.4367P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1221
_refine_ls_wR_factor_ref         0.1303
_reflns_number_gt                20668
_reflns_number_total             26062
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b919934a.txt
_cod_data_source_block           kpo_3_273dmas
_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 2.4.2 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      P2(1)/c
_cod_database_code               7212119