Tungsten oxide as a universal source for the synthesis of complexes with different nuclearities in WO<sub>3</sub>/chalcogen/NaCN systems.
Yarovoy, Spartak S.; Mirzaeva, Irina V.; Sukhikh, Taisiya S.; Mironov, Yuri V.; Yanshole, Vadim; Brylev, Konstantin A.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 8644–8657; doi:10.1039/d5dt00361j

data_7718620
_publ_section_title
;
 Tungsten oxide as a universal source for the synthesis of complexes with
 different nuclearities in WO<sub>3</sub>/chalcogen/NaCN systems.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8644
_journal_page_last               8657
_journal_paper_doi               10.1039/d5dt00361j
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C9 Cs3.5 N9 Na1.5 Se4 W3, 6.5(O H2)'
_chemical_formula_sum            'C9 H13 Cs3.5 N9 Na1.5 O6.5 Se4 W3'
_chemical_formula_weight         1713.95
_space_group_crystal_system      trigonal
_space_group_IT_number           166
_space_group_name_Hall           '-R 3 2"'
_space_group_name_H-M_alt        'R -3 m :H'
_atom_sites_solution_primary     dual
_audit_creation_date             2024-10-04
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-10-22 deposited with the CCDC.	2025-04-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   11.7075(5)
_cell_length_b                   11.7075(5)
_cell_length_c                   44.409(3)
_cell_measurement_reflns_used    5262
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      2.21
_cell_volume                     5271.4(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 8.33
_diffrn_detector_type            'Bruker APEXII CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       -57
_diffrn_reflns_number            12140
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.556
_diffrn_reflns_theta_min         2.060
_diffrn_source                   'sealed tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    17.529
_exptl_absorpt_correction_T_max  0.0468
_exptl_absorpt_correction_T_min  0.0165
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0891 before and 0.0524 after correction.
The Ratio of minimum to maximum transmission is 0.3526.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    3.215
_exptl_crystal_description       plate
_exptl_crystal_F_000             4406
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.852
_refine_diff_density_min         -1.972
_refine_diff_density_rms         0.385
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     73
_refine_ls_number_reflns         1557
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.136
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0558
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1016P)^2^+350.9702P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1687
_refine_ls_wR_factor_ref         0.1860
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1288
_reflns_number_total             1557
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00361j2.cif
_cod_data_source_block           ys1222
_cod_depositor_comments
'Adding full bibliography for 7718618--7718621.cif.'
_cod_original_cell_volume        5271.4(6)
_cod_original_sg_symbol_H-M      'R -3 m'
_cod_original_formula_sum        'C9 Cs3.5 H13 N9 Na1.5 O6.5 Se4 W3'
_cod_database_code               7718620
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.334
_shelx_estimated_absorpt_t_min   0.102
_olex2_refinement_description
;
1. Shared sites
{O2, Cs2}
2. Uiso/Uaniso restraints and constraints
Uanis(O2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O2) = Uanis(Cs2)
3. Others
 Sof(Cs2)=0.25*(1-FVAR(2))
 Sof(O2)=0.25*FVAR(2)
 Fixed Sof: O1(0.25) O7(0.5)
;
_shelx_res_checksum              81283
_shelx_hkl_checksum              57913
_olex2_submission_special_instructions 'No special instructions were received'