Cyclic Tungstoselenites Based on {Se2W12} Units.
Kalinina, Irina V.; Peresypkina, Eugenia V.; Izarova, Natalya V.; Nkala, Fiona M.; Kortz, Ulrich; Kompankov, Nikolay B.; Moroz, Nikolay K.; Sokolov, Maxim N.; Inorganic chemistry 53 (2014) 2076–2082; doi:10.1021/ic402668v

data_4337233
_publ_section_title
;
 Cyclic Tungstoselenites Based on {Se2W12} Units.
;
_journal_issue                   4
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2076
_journal_page_last               2082
_journal_paper_doi               10.1021/ic402668v
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety
'2K +, 22Na +, (O144 Se6 W39) 24-, 57.75(H2 O)'
_chemical_formula_structural
'K2 Na22 [(Se2 W12 O46 (WO(H2 O)))3] * 57.75(H2 O)'
_chemical_formula_sum            'H60.75 K2 Na22 O201.75 Se6 W39'
_chemical_formula_weight         11517.13
_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   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                88.1380(10)
_cell_angle_beta                 79.1710(10)
_cell_angle_gamma                75.0520(10)
_cell_formula_units_Z            2
_cell_length_a                   14.1423(2)
_cell_length_b                   22.4551(3)
_cell_length_c                   35.5982(4)
_cell_measurement_reflns_used    43062
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      29.6355
_cell_measurement_theta_min      4.1942
_cell_volume                     10726.2(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 7.9851
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0634
_diffrn_reflns_av_sigmaI/netI    0.1401
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            181828
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.70
_diffrn_reflns_theta_min         4.20
_exptl_absorpt_coefficient_mu    22.026
_exptl_absorpt_correction_T_max  0.702
_exptl_absorpt_correction_T_min  0.215
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.566
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             10090
_exptl_crystal_size_max          0.1020
_exptl_crystal_size_mid          0.0597
_exptl_crystal_size_min          0.0193
_refine_diff_density_max         3.109
_refine_diff_density_min         -2.048
_refine_diff_density_rms         0.291
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.774
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2693
_refine_ls_number_reflns         56584
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.774
_refine_ls_R_factor_all          0.0848
_refine_ls_R_factor_gt           0.0373
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0237P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0684
_refine_ls_wR_factor_ref         0.0724
_reflns_number_gt                29329
_reflns_number_total             56584
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402668v_si_003.cif
_cod_data_source_block           1b
_cod_database_code               4337233