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_4309881
_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            'C6 H15 I2.5 K3 Mo3 N7.5 O4.5 Se7'
_chemical_formula_weight         1539.35
_space_group_IT_number           165
_symmetry_cell_setting           rhombohedral
_symmetry_Int_Tables_number      165
_symmetry_space_group_name_Hall  '-P 3 2"c'
_symmetry_space_group_name_H-M   'P -3 c 1'
_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                120.00
_cell_formula_units_Z            4
_cell_length_a                   12.9160(15)
_cell_length_b                   12.9160(15)
_cell_length_c                   23.080(6)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13.85
_cell_measurement_theta_min      10.64
_cell_volume                     3334.4(10)
_computing_cell_refinement       'CD4CA0 (Enraf-Nonius, 1989)'
_computing_data_collection       'CD4CA0 (Enraf-Nonius, 1989)'
_computing_data_reduction        'CADDAT (Enraf-Nonius, 1989)'
_computing_molecular_graphics    'ORTEP-III (Burnett & Johnson, 1996)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       2\q/\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0546
_diffrn_reflns_av_sigmaI/netI    0.0670
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3891
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         1.76
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    11.470
_exptl_absorpt_correction_T_max  0.2075
_exptl_absorpt_correction_T_min  0.1079
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'CADDAT (Enraf-Nonius, 1989)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    3.066
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2772
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.783
_refine_diff_density_min         -1.036
_refine_diff_density_rms         0.273
_refine_ls_extinction_coef       0
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         1967
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      0.966
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0423
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0685P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1112
_refine_ls_wR_factor_ref         0.1185
_reflns_number_gt                1408
_reflns_number_total             1967
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050962csi20050614_030518.cif
_cod_data_source_block           pa21
_cod_original_formula_sum        'C6 H15 I2.50 K3 Mo3 N7.50 O4.50 Se7'
_cod_database_code               4309881