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_4337232
_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
'(H12 Cl Mn4 O100 Se6 W24) 13-, 51(H2 O), 13(Na)+'
_chemical_formula_structural
'Na13 [(Se2 W12 O46)2 {Mn2 Cl (H2 O)2} {Mn (H2O)2}2 (Se O)2] * 51(H2 O)'
_chemical_formula_sum            'Cl H112 Mn4 Na13 O151 Se6 W24'
_chemical_formula_weight         7969.14
_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                77.1050(10)
_cell_angle_beta                 69.9680(10)
_cell_angle_gamma                66.6280(10)
_cell_formula_units_Z            1
_cell_length_a                   13.9680(4)
_cell_length_b                   15.6454(5)
_cell_length_c                   18.3497(5)
_cell_measurement_reflns_used    8432
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      37.7731
_cell_measurement_theta_min      2.4802
_cell_volume                     3440.57(18)
_computing_cell_refinement       'Apex2 V.1.27 (Bruker, 2005)'
_computing_data_collection       'Apex2 V.1.27 (Bruker, 2005)'
_computing_data_reduction        'Apex2 V.1.27 (Bruker, 2005)'
_computing_molecular_graphics    'SHELXTL V6.22 (Bruker, 2000-2005)'
_computing_publication_material  'local programs'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector_area_resol_mean 25
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.882
_diffrn_measurement_device_type  'Bruker X8Apex CCD detector'
_diffrn_measurement_method       'combined omega- and phi-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  0.0362
_diffrn_reflns_av_sigmaI/netI    0.0861
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            47249
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         38.21
_diffrn_reflns_theta_min         1.66
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    22.098
_exptl_absorpt_correction_T_max  0.7475
_exptl_absorpt_correction_T_min  0.6029
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'based on intensities (SADABS, Bruker, 2005)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.846
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3560
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         3.431
_refine_diff_density_min         -2.836
_refine_diff_density_rms         0.539
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     945
_refine_ls_number_reflns         33528
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0872
_refine_ls_R_factor_gt           0.0469
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0256P)^2^+8.8575P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0800
_refine_ls_wR_factor_ref         0.0915
_reflns_number_gt                22796
_reflns_number_total             33528
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402668v_si_004.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        3440.57(17)
_cod_original_formula_sum        'H112 Cl Mn4 Na13 O151 Se6 W24'
_cod_database_code               4337232