Synthesis and Reactivity of W3Te74+ Clusters and Chalcogen Exchange in the M3Q7 (M = Mo, W; Q = S, Se, Te) Cluster Family
Maxim N. Sokolov; Pavel A. Abramov; Artem L. Gushchin; Irina V. Kalinina; Dmitry Y. Naumov; Alexander V. Virovets; Eugenia V. Peresypkina; Cristian Vicent; Rosa Llusar; Vladimir P. Fedin; Inorganic Chemistry 44 (2005) 8116–8124; doi:10.1021/ic050962c

data_4309878
_publ_contact_author_address
;Nikolaev Institute of Inorganic Chemistry,
SB Russian Academy of Sciences,
Academition Lavrentiev Avenue 3,
Novosibirsk 90,
630090 Russia
;
_publ_contact_author_email       d.y.naumov@ngs.ru
_publ_contact_author_fax         7(3832)344489
_publ_contact_author_name        'Dr. Dmitry Yu. Naumov'
_publ_contact_author_phone       7(3832)344466
_publ_section_title
;
Synthesis and Reactivity of W3Te74+ Clusters and Chalcogen Exchange in the
M3Q7 (M = Mo, W; Q = S, Se, Te) Cluster Family
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8116
_journal_page_last               8124
_journal_paper_doi               10.1021/ic050962c
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C12 H10 Cl2 Cs2 K4 N12 O5 Te14 W6'
_chemical_formula_weight         3784.94
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   25.626(9)
_cell_length_b                   60.07(2)
_cell_length_c                   15.614(5)
_cell_measurement_reflns_used    2565
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      19.1824
_cell_measurement_theta_min      2.2817
_cell_volume                     24035(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 25
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker-Nonius X8Apex CCD'
_diffrn_measurement_method       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  0.1003
_diffrn_reflns_av_sigmaI/netI    0.1624
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       78
_diffrn_reflns_limit_k_min       -57
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            30466
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.36
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    19.696
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.339156
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'based on intensities (SADABS)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    4.184
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'lath-shaped, close to needle'
_exptl_crystal_F_000             25568
_exptl_crystal_size_max          0.0075
_exptl_crystal_size_mid          0.0125
_exptl_crystal_size_min          0.25
_refine_diff_density_max         2.651
_refine_diff_density_min         -1.531
_refine_diff_density_rms         0.341
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.011(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.846
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     528
_refine_ls_number_reflns         11569
_refine_ls_number_restraints     181
_refine_ls_restrained_S_all      0.844
_refine_ls_R_factor_all          0.1161
_refine_ls_R_factor_gt           0.0544
_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^)+(0.0556P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1173
_refine_ls_wR_factor_ref         0.1304
_reflns_number_gt                5838
_reflns_number_total             11569
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050962csi20050614_030308.cif
_cod_data_source_block           ag228-2
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '_atom_site_symetry_multiplicity' was replaced with
'_atom_site_symmetry_multiplicity' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_cell_volume        24037(14)
_cod_database_code               4309878