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_7718621
_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 Cs2.75 N9 Na2.25 S4 W3, 2.25(H2 O)'
_chemical_formula_sum            'C9 H4.5 Cs2.75 N9 Na2.25 O2.25 S4 W3'
_chemical_formula_weight         1371.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_primary     dual
_audit_creation_date             2024-10-21
_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                 108.9850(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.4777(6)
_cell_length_b                   11.2976(4)
_cell_length_c                   13.2992(4)
_cell_measurement_reflns_used    9985
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.14
_cell_measurement_theta_min      2.87
_cell_volume                     2767.31(16)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_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                 PIXEL
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Incoatec HELIOS multilayer mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20480
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.153
_diffrn_reflns_theta_min         2.115
_diffrn_source                   'Incoatec IuS3.0 microfocus X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    16.368
_exptl_absorpt_correction_T_max  0.1044
_exptl_absorpt_correction_T_min  0.0488
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1242 before and 0.0599 after correction.
The Ratio of minimum to maximum transmission is 0.4674.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark violet'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    3.282
_exptl_crystal_description       plate
_exptl_crystal_F_000             2388
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.934
_refine_diff_density_min         -3.000
_refine_diff_density_rms         0.290
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         5518
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0352P)^2^+37.4147P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0858
_refine_ls_wR_factor_ref         0.0890
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4894
_reflns_number_total             5518
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00361j2.cif
_cod_data_source_block           ys2239
_cod_depositor_comments
'Adding full bibliography for 7718618--7718621.cif.'
_cod_database_code               7718621
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.853
_shelx_estimated_absorpt_t_min   0.354
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(Cs1) = Uanis(O1)
2. Others
 Fixed Sof: Cs1(0.375) Cs2(0.5) Na2(0.375) O1(0.125) O2(0.5)
;
_shelx_res_checksum              34091
_shelx_hkl_checksum              7470
_olex2_submission_special_instructions 'No special instructions were received'