From oxide to a new type of molecular tungsten compound: formation of bitetrahedral cluster complexes [{W<sub>6</sub>(μ<sub>4</sub>-O)<sub>2</sub>(μ<sub>3</sub>-CCN)<sub>4</sub>}(CN)<sub>16</sub>]<sup>10-</sup> and [{W<sub>6</sub>(μ<sub>4</sub>-O)<sub>2</sub>(μ<sub>3</sub>-As)<sub>4</sub>}(CN)<sub>16</sub>]<sup>10</sup>.
Yarovoy, Spartak S.; Smolentsev, Anton I.; Kozlova, Svetlana G.; Kompankov, Nikolay B.; Gayfulin, Yakov M.; Asanov, Igor P.; Yanshole, Vadim V.; Mironov, Yuri V.; Chemical communications (Cambridge, England) 54 (2018) 13837–13840; doi:10.1039/c8cc07746k

data_7122628
_publ_section_title
;
 From oxide to a new type of molecular tungsten compound: formation of
 bitetrahedral cluster complexes
 [{W<sub>6</sub>(\m<sub>4</sub>-O)<sub>2</sub>(\m<sub>3</sub>-CCN)<sub>4</sub>}(CN)<sub>16</sub>]<sup>10-</sup>
 and
 [{W<sub>6</sub>(\m<sub>4</sub>-O)<sub>2</sub>(\m<sub>3</sub>-As)<sub>4</sub>}(CN)<sub>16</sub>]<sup>10</sup>.
;
_journal_issue                   98
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              13837
_journal_page_last               13840
_journal_paper_doi               10.1039/c8cc07746k
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C24 N20 O2 W6, 11(H2 O), 10(K)'
_chemical_formula_sum            'C24 H22 K10 N20 O13 W6'
_chemical_formula_weight         2292.72
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2018-08-30 deposited with the CCDC.
2018-11-15 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 126.841(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.8574(5)
_cell_length_b                   16.6740(5)
_cell_length_c                   22.6906(5)
_cell_measurement_reflns_used    9988
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.44
_cell_volume                     5407.0(3)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2004)'
_computing_publication_material  'SHELXTL (Bruker, 2004)'
_computing_structure_refinement  'SHELXTL (Bruker, 2004)'
_computing_structure_solution    'SHELXTL (Bruker, 2004)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 25
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Nonius X8Apex CCD area-detector'
_diffrn_measurement_method       '\f and \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  0.0495
_diffrn_reflns_av_sigmaI/netI    0.0507
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            47393
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         1.66
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    13.553
_exptl_absorpt_correction_T_max  0.5506
_exptl_absorpt_correction_T_min  0.1156
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2004)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.816
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4176
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.116
_refine_diff_density_min         -2.828
_refine_diff_density_rms         0.279
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_matrix_type           full
_refine_ls_number_parameters     658
_refine_ls_number_reflns         12439
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0348
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0339P)^2^+14.7528P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0779
_refine_ls_wR_factor_ref         0.0836
_reflns_number_gt                9623
_reflns_number_total             12439
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8cc07746k2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7122628--7122629.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7122628