Two Keggin sandwich-type tungstophosphates modified by open-chain carboxyethyltin groups and transition metals
Zhang, Bai; Zhang, Lan-Cui; Zhang, Yajun; Su, fang; You, wansheng; Zhu, Zaiming; RSC Adv.  (2015) –; doi:10.1039/C5RA07419C

data_7220532
_publ_section_title
;
 Two Keggin sandwich-type tungstophosphates modified by open-chain
 carboxyethyltin groups and transition metals
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA07419C
_journal_year                    2015
_chemical_formula_moiety         'C6 H8 K2 Na8 O72 P2 Sn2 W18 Zn2,13H2O'
_chemical_formula_sum            'C6 H34 K2 Na8 O85 P2 Sn2 W18 Zn2'
_chemical_formula_weight         5467.81
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-04-17 deposited with the CCDC.
2015-05-19 downloaded from the CCDC.
;
_cell_angle_alpha                96.179(3)
_cell_angle_beta                 104.324(2)
_cell_angle_gamma                119.353(2)
_cell_formula_units_Z            1
_cell_length_a                   12.2118(17)
_cell_length_b                   12.401(2)
_cell_length_c                   15.826(2)
_cell_measurement_reflns_used    6078
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.59
_cell_measurement_theta_min      1.93
_cell_volume                     1948.3(5)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997a)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997b)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997b)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker Apex2 CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0575
_diffrn_reflns_av_sigmaI/netI    0.1129
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9870
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    27.997
_exptl_absorpt_correction_T_max  0.3790
_exptl_absorpt_correction_T_min  0.1944
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    4.660
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2398
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         3.345
_refine_diff_density_min         -5.644
_refine_diff_density_rms         0.612
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     572
_refine_ls_number_reflns         6826
_refine_ls_number_restraints     155
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1061
_refine_ls_R_factor_gt           0.0770
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1288P)^2^+7.5343P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1966
_refine_ls_wR_factor_ref         0.2194
_reflns_number_gt                4890
_reflns_number_total             6826
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ra07419c2.cif
_cod_data_source_block           1
_cod_original_cell_volume        1948.2(5)
_cod_database_code               7220532